CN114621079A - Method for extracting long-chain dicarboxylic acid from fermentation liquor - Google Patents
Method for extracting long-chain dicarboxylic acid from fermentation liquor 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
- B01D36/04—Combinations of filters with settling tanks
- B01D36/045—Combination of filters with centrifugal separation devices
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Abstract
The invention provides a method for extracting long-chain dibasic acid from fermentation liquor, which is characterized in that for the fermentation liquor with the ph of 6.5-7.5 and the temperature of 28-30 ℃, the long-chain dibasic acid in the fermentation liquor mainly exists in a crystal form, and the steps of primary centrifugation, primary water adding and pulp mixing, secondary centrifugation, secondary water adding and pulp mixing, filter pressing and drying are adopted to realize the extraction of a long-chain dibasic acid finished product from the fermentation liquor. Compared with the traditional long-chain binary acid extraction process, the method does not need to use a large amount of strong acid and strong base in the production, so that the content of sodium sulfate in the wastewater is low, the treatment cost is low, the environment is protected, the long-chain binary acid can be separated from impurities such as thalli and the like through a horizontal spiral centrifugal machine, water, electricity and steam are saved in the production, a cleaning agent is not needed, the equipment investment is lower, the economic benefit is obvious, and the industrial mass production is facilitated.
Description
Technical Field
The invention relates to a method for preparing long-chain dibasic acid by a biological fermentation method, in particular to a method for extracting long-chain dibasic acid from fermentation liquor.
Background
The long-chain dibasic acid is generally an organic compound having a carboxyl group at both ends of a straight carbon chain, and a dibasic acid having more than ten carbon atoms is conventionally referred to as a long-chain dibasic acid. In the national economic classification, long-chain dibasic acids belong to the chemical raw material and chemical product manufacture in the manufacturing industry in the large category of the national economic classification, and the subdivision subclass is the organic chemical raw material manufacture in the basic chemical raw material manufacture.
The long-chain binary acid is an important intermediate raw material in the chemical process, and is a main raw material for synthesizing special products such as musk-T, copolyamide hot melt adhesive, nylon, engineering plastics and the like. The long-chain dibasic acid is used as a basic raw material to produce and synthesize fine chemical products such as high-grade spice musk, high-grade nylon rubber, high-temperature electrolyte, high-grade hot melt adhesive, cold-resistant plasticizer, high-grade lubricating oil, high-grade paint, coating and the like, and the method is widely applied to the fields of chemical industry, light industry, pesticide, medicine, liquid crystal material, military industry and the like.
Due to wide application of the long-chain dicarboxylic acid, the downstream product has excellent performance and wide development potential. The demand of long-chain dibasic acid is increasing at home and abroad, and the market potential is very large.
The traditional long-chain dibasic acid extraction technology is that liquid alkali is added into fermentation liquor, the pH value of the fermentation liquor is adjusted to 9-11 from 6-7, long-chain dibasic acid is dissolved in water in the form of dibasic acid sodium salt, the temperature is raised to more than 70 ℃, thalli and other impurities are removed through membrane filtration, concentrated sulfuric acid is added into obtained filtrate, a method of replacing weak acid with strong acid is used for extracting a dibasic acid product, and after membrane filtration is finished, a cleaning agent and softened water are used for cleaning a membrane group to ensure the filtration performance of the product. Dangerous chemicals such as strong acid, strong base, cleaning agent and the like are required in the production of the method, the consumption of water, electricity and steam is high, the amount of discharged wastewater is large, sodium sulfate contained in the wastewater is difficult to treat, the equipment price is high, and the investment is large.
Disclosure of Invention
The invention provides a method for extracting long-chain dibasic acid from fermentation liquor with the pH value of 6.5-7.5 and the temperature of lower than 30 ℃, which effectively solves the problems that dangerous chemicals such as strong acid, strong alkali, cleaning agent and the like are required to be used, the energy consumption and the waste discharge are high, sodium sulfate is difficult to treat, the equipment cost is high and the like, wherein the prepared long-chain dibasic acid comprises one or more long-chain dibasic acids of C10-C18. The technical scheme is as follows:
a method for extracting long-chain dicarboxylic acid from fermentation liquor comprises the following steps:
s1: inputting the fermented liquid into a fermented liquid storage tank after fermentation;
s2: primary centrifugation: conveying the fermentation liquor into a first horizontal spiral centrifuge by a fermentation liquor storage tank to obtain a long-chain dibasic acid solid phase and a liquid phase mainly containing thalli, inputting the long-chain dibasic acid solid phase into a first slurry mixing tank, and inputting the liquid phase mainly containing thalli into a mother liquor tank;
s3: adding water for primary size mixing: adding normal-temperature softened water into the first slurry mixing tank, starting the first slurry mixing tank to stir after the long-chain dicarboxylic acid solid phase enters the first slurry mixing tank, and forming a long-chain dicarboxylic acid solid-liquid mixed material;
s4: and (3) secondary centrifugation: conveying the long-chain dicarboxylic acid solid-liquid mixed material in the first slurry mixing tank into a second horizontal spiral centrifugal machine to obtain a long-chain dicarboxylic acid solid phase and a liquid phase containing a small amount of thalli, and conveying the liquid phase containing the small amount of thalli into a mother liquor tank;
s5: and (3) secondary water adding and size mixing: conveying the long-chain dicarboxylic acid solid phase to a second slurry mixing tank by a second horizontal spiral centrifuge, adding normal-temperature softened water into the second slurry mixing tank, and opening the second slurry mixing tank to stir after the long-chain dicarboxylic acid solid phase enters the second slurry mixing tank to form a long-chain dicarboxylic acid solid-liquid mixed material;
s6: and (3) filter pressing: and conveying the long-chain dicarboxylic acid solid-liquid mixed material in the second slurry mixing tank into a plate-and-frame filter press, cleaning, squeezing and blow-drying to obtain a long-chain dicarboxylic acid solid phase.
Further, the method includes step S7: and (3) drying: and conveying the long-chain dibasic acid solid phase subjected to filter pressing into a flash evaporation dryer through a screw conveyor, and drying to obtain a long-chain dibasic acid finished product with the purity of more than 97% and the moisture of less than 0.3%.
Further, in step S1, the pH of the fermentation broth is 6.5 to 7.5, and the temperature is 28 ℃ to 30 ℃.
Further, the rotating speed of the first horizontal type spiral centrifugal machine in the step S2 is 1000r/min-1300r/min during operation; and the rotating speed of the second horizontal spiral centrifugal machine in the step S4 is 2000r/min-5000r/min during operation.
Further, in step S3, the ratio of the water content to the solid phase in the long-chain dicarboxylic acid solid-liquid mixture is 1:1 to 2: 1.
Further, in step S4, sampling and inspecting the long-chain dibasic acid solid phase output by the second horizontal screw centrifuge, and when the total nitrogen content of the long-chain dibasic acid solid phase is not more than 0.01%, directly conveying the long-chain dibasic acid solid phase to a screw conveyor, and performing drying treatment in step S7; and when the total nitrogen content of the long-chain dibasic acid solid phase is higher than 0.01%, conveying the long-chain dibasic acid solid phase to a second slurry mixing tank, and continuing to process in the following step S5.
Further, in step S5, the ratio of the water content to the solid phase in the long-chain dicarboxylic acid solid-liquid mixture is 1:1-2: 1. Particularly, the ratio of water to solid phase in the long-chain dicarboxylic acid solid-liquid mixed material is 1.5: 1.
Further, the secondary centrifugation of step S4 and the secondary water-adding and pulp-mixing of step S5 can be repeatedly used a plurality of times before step S6 as a combination for removing impurities.
A product produced according to the method of extracting long chain dibasic acids from a fermentation broth, the product comprising one or more of the long chain dibasic acids of C10-C18.
The method for extracting the long-chain dicarboxylic acid from the fermentation liquor provided by the invention has the advantages that hazardous chemicals such as strong acid, strong base and the like are not used in all processes, the fermentation liquor is not required to be heated, the production can be completed under the conditions that the pH value of the fermentation liquor is 6.5-7.5 and the temperature is 28-30 ℃, the use of the hazardous chemicals such as the strong acid, the strong base and the like can be reduced, the discharge amount of waste water and the content of sodium sulfate in the waste water are reduced, further, the application environment for separating the long-chain dicarboxylic acid from thalli can reduce the consumption of water, electricity and steam, the equipment investment is less, the industrial amplification production is facilitated, the waste water treatment cost is lower, and the production is more environment-friendly.
Drawings
FIG. 1 is a process flow diagram of the method for extracting long-chain dicarboxylic acid from the fermentation broth;
FIG. 2 is a process flow diagram of the current method.
Detailed Description
As shown in figure 1, the method for extracting the long-chain dibasic acid from the fermentation liquor uses extraction equipment comprising a fermentation liquor storage tank 1, a first horizontal spiral centrifuge 3, a first slurry mixing tank 4, a second horizontal spiral centrifuge 7, a second slurry mixing tank 8, a plate-and-frame filter press 10, a spiral conveyor 12 and a flash dryer 13 which are connected in sequence. The plate-and-frame filter press 10 is connected to a sewage treatment plant 11, the fermentation liquor storage tank 1 is used for inputting fermentation liquor, and the flash evaporation dryer 13 is used for outputting finished products.
A first centrifugal pump 2 is arranged between the fermentation liquor storage tank 1 and the first horizontal spiral centrifuge 3, a second centrifugal pump 5 is arranged between the first slurry mixing tank 4 and the second horizontal spiral centrifuge 7, a third centrifugal pump 9 is arranged between the second slurry mixing tank 8 and the plate-and-frame filter press 10, and the first horizontal spiral centrifuge 3 and the second horizontal spiral centrifuge 7 are both connected with a mother liquor tank 6.
A first valve 21 is arranged on a pipeline between the first horizontal screw centrifuge 3 and the first slurry mixing tank 4, a second valve 22 and a third valve 23 are arranged on a pipeline between the second horizontal screw centrifuge 7 and the second slurry mixing tank 8, a branch pipeline communicated with the screw conveyor 12 is arranged on a pipeline between the second valve 22 and the third valve 23, a fourth valve 24 is arranged on the branch pipeline, and a sampling valve 25 is arranged between the second horizontal screw centrifuge 7 and the second valve 22.
Example 1
The invention will be further described with reference to the accompanying drawings and specific embodiments so that those skilled in the art may better understand the invention, but the invention is not limited thereto.
In fig. 1, the power of the first horizontal screw centrifuge 3 is 70.5kW · h, and the power of the second horizontal screw centrifuge 7 is 37.5kW · h. The volumes of the first slurry mixing tank 4 and the second slurry mixing tank 8 are bothIs 6m3. The liquid phase mentioned in the invention mainly contains water, thallus, and also contains a small amount of other impurities and dodecanedioic acid (the long-chain diacid mentioned in the examples and comparative examples refers to C12 long-chain diacid).
In combination with the above extraction apparatus, the present invention comprises the steps of:
s1: the fermentation liquid after fermentation enters a fermentation liquid storage tank 1 under pressure, the pH value of the fermentation liquid is 7.2, the temperature is 29.5 ℃, and the volume is 180m3；
S2: primary centrifugation: conveying the fermentation liquor into a first horizontal spiral centrifuge 3 by using a first centrifugal pump 2, regulating and maintaining the rotating speed of the first horizontal spiral centrifuge 3 at 1250r/min, centrifuging to obtain a long-chain dibasic acid solid phase and a liquid phase mainly containing thalli, feeding the liquid phase into a mother liquor tank 6 through a pipeline, opening a first valve 21, and feeding the solid phase into a first slurry mixing tank 4 through a pipeline;
s3: adding water for primary size mixing: adding room temperature softened water 3m into the first size mixing tank 43After the long-chain dicarboxylic acid solid phase enters the first slurry mixing tank 4 through a pipeline, the first slurry mixing tank 4 is started to stir so that water and the long-chain dicarboxylic acid solid phase are fully mixed to form a long-chain dicarboxylic acid solid-liquid mixed material, and the long-chain dicarboxylic acid solid-liquid mixed material is continuously fed until the length of the long-chain dicarboxylic acid solid-liquid mixed material is 5m3When the material is discharged, the first valve 21 is closed to stop discharging;
the purpose of the step is as follows: and the long-chain dicarboxylic acid after the primary centrifugation is rinsed by water, so that the long-chain dicarboxylic acid, thalli and other impurities can be conveniently separated in the next step, and the second centrifugal pump 5 can conveniently convey materials.
S4: and (3) secondary centrifugation: and (3) conveying the long-chain dicarboxylic acid solid-liquid mixed material in the first slurry mixing tank 4 into a second horizontal spiral centrifugal machine 7 by using a second centrifugal pump 5, opening a first valve 21 after the solid-liquid mixed material in the slurry mixing tank is conveyed, and repeating the process of adding water and mixing slurry for one time.
And adjusting and maintaining the rotation speed of the second horizontal spiral centrifuge 7 at 4000r/min, centrifuging to obtain a long-chain dicarboxylic acid solid phase and a liquid phase containing a small amount of thalli, feeding the liquid phase containing the small amount of thalli into the mother liquor tank 6 through a pipeline, taking the solid phase from the sampling valve 25, detecting to obtain the total nitrogen content of 0.03%, opening the second valve 22 and the third valve 23, closing the fourth valve 24, and feeding the solid phase into the second slurry mixing tank 8 through a pipeline.
Thalli and other impurities in the long-chain dibasic acid are further removed through secondary centrifugation, the purity of the long-chain dibasic acid is improved, and whether the thalli are removed qualified or not is checked through measuring the total nitrogen content of a solid phase.
S5: and (3) secondary water adding and size mixing: adding room temperature softened water 3m into the second slurry mixing tank 83After the long-chain dicarboxylic acid solid phase enters a second slurry mixing tank 8 through a pipeline, starting the slurry mixing tank to stir so that water and the long-chain dicarboxylic acid solid are fully mixed to form a long-chain dicarboxylic acid solid-liquid mixed material, and continuously feeding the long-chain dicarboxylic acid solid-liquid mixed material until the length of the long-chain dicarboxylic acid solid-liquid mixed material is 5m3When the second valve 22 and the third valve 23 are closed.
The purpose of the step is as follows: and (4) continuously rinsing the centrifuged long-chain dibasic acid with water, so that the long-chain dibasic acid with high total nitrogen content is conveniently separated from the thalli in the next step.
S6: and (3) filter pressing: and (3) conveying the long-chain dicarboxylic acid solid-liquid mixed material in the second slurry mixing tank 8 into a plate-and-frame filter press 10 by using a third centrifugal pump 9, opening a second valve 22 and a third valve 23 after the solid-liquid mixed material is conveyed, and repeating the process of adding water and mixing slurry for the second time.
The long-chain dicarboxylic acid solid-liquid mixed material is cleaned, filter-pressed and blow-dried by a plate-and-frame filter press 10, and then is discharged by pulling a plate, and the obtained long-chain dicarboxylic acid solid phase directly enters a screw conveyor 12.
The purpose of the step is as follows: the long-chain dibasic acid solid-liquid mixed material is washed and filter-pressed by a plate-and-frame filter press 10, and other impurities such as a small amount of bacteria contained in the long-chain dibasic acid are thoroughly removed.
S7: and (3) drying: the solid phase of the long-chain dibasic acid is sent into a flash evaporation dryer 13 through a screw conveyor 12, and a long-chain dibasic acid finished product with the purity of 97.2 percent and the moisture of 0.28 percent is obtained after drying.
Example 2
The fermentation broth after fermentation is fed into a fermentation broth storage tank 1 under pressure, the pH value of the fermentation broth is 6.9, the temperature is 29.0 ℃, and the volume is 180m3。
The steps of the primary centrifugation, the primary water adding and pulp mixing and the secondary centrifugation are consistent with the steps of the embodiment 1, the long-chain dicarboxylic acid solid phase after the secondary centrifugation is taken from the sampling valve and is detected, the total nitrogen content is detected to be 0.008 percent, the second valve 22 and the fourth valve 24 are opened, the third valve 23 is closed, and the long-chain dicarboxylic acid solid phase enters the screw conveyer 12 through a pipeline.
S7: and (3) drying: the long-chain dicarboxylic acid solid phase is sent into a flash evaporation dryer 13 through a screw conveyor 12, and a long-chain dicarboxylic acid finished product with the purity of 97.7 percent and the moisture of 0.2 percent is obtained after drying.
In the method, the secondary centrifugation of the step S4 and the secondary water adding and pulp mixing of the step S5 can be repeatedly used for a plurality of times before the step S6 as the combination for removing impurities.
Comparative example 1 (current process):
as shown in fig. 2, the extraction equipment used in the present method includes a fermentation liquid storage tank 1, a membrane filtration equipment 14, a decolorization tank 15, a relay plate-and-frame filter press 16, a buffer tank 17, a neutralization tank 19, a plate-and-frame filter press 10, a screw conveyor 12, and a flash dryer 13, which are connected in sequence. The plate-and-frame filter press 10 is connected to a sewage treatment plant 11, the fermentation liquor storage tank 1 is used for inputting fermentation liquor and liquid caustic soda, and the flash evaporation dryer 13 is used for outputting finished products.
A first centrifugal pump 2 is arranged between the fermentation liquor storage tank 1 and the membrane filtering equipment 14, the membrane filtering equipment 14 is also provided with a pipeline leading to the input end of the fermentation liquor storage tank 1, a second centrifugal pump 5 is arranged between the decoloring tank 15 and the relay plate and frame filter press 16, the relay plate and frame filter press 16 needs to be subjected to waste carbon treatment, a fourth centrifugal pump 18 is arranged between the buffer tank 17 and the neutralization tank 19, the neutralization tank 19 needs to be fed with water and concentrated sulfuric acid, and a fifth centrifugal pump 20 is arranged between the neutralization tank 19 and the plate and frame filter press 10.
When the process of the prior method is adopted to extract the long-chain dicarboxylic acid from the fermentation liquor, 180m is needed to be firstly extracted3Adjusting pH of the fermentation liquid from 6-7, adding alkali to 9-10, consuming alkali about 5.6T, heating the fermentation liquid from 30 ℃ to 70 ℃, and consuming saturated steam of 0.5MPa about 11T.
In the traditional method, in the filtration production process, along with the precipitation of thalli and the concentration of fermentation liquor, water needs to be added step by step for dilutionThe filtration is completed, and the total amount of the filter medium is 100m3The production water with the temperature of 70 ℃ consumes about 6T of 0.5MPa saturated steam when the temperature is raised.
After the production of the membrane filtration, 35m is needed for washing the membrane group for many times by using a cleaning agent and softened water3Softened water with a temperature of 70 ℃ and 50m of produced water3The cleaning agent 450KG is needed, the temperature rise consumes about 2T of 0.5MPa saturated steam, the cleaning time is 4h, if the membrane blockage causes the poor filtering effect, the filtration needs to be stopped, the membrane group is cleaned, and the filtering time and the water consumption are further increased.
The main power consumption equipment in the traditional method production is a membrane filtration system, the system also comprises 2 132 kW.h circulating pumps and 130 kW.h secondary feeding pump, and the power consumption per hour is 294 kW.h.
In the traditional method, 17T concentrated sulfuric acid and 50m of concentrated sulfuric acid are added into a neutralization tank 19 in production3Producing water, replacing weak acid with strong acid, heating the feed liquid to 90 deg.C, recrystallizing with crystal to obtain solid-liquid mixture of long-chain dicarboxylic acid, and consuming 0.5MPa saturated steam about 27T.
The data combined are compared as follows:
the following can be found by combining the above tables: by using the method of the invention, the water consumption in the production is only the water for size mixing, about 96m3Softened water, converted to produced water 137m3Because the working principle is spiral sedimentation, a large amount of water and cleaning agent are not needed to flush after the operation is finished, and the traditional method consumes 200m of production water in production3(ii) a Therefore, the method reduces the water consumption by 31.5 percent, thereby greatly reducing the sewage discharge in the production.
By using the method, strong acid, strong alkali and cleaning agent are not needed in the production, so that the auxiliary material cost can be reduced, the content of sodium sulfate in the wastewater can be greatly reduced, the sewage treatment cost is reduced, and the method is more environment-friendly.
The main equipment in the method is that the power of two horizontal spiral centrifuges is respectively 70.5 kW.h and 37.5 kW.h, and the electricity consumption per hour is 108 kW.h; the traditional method mainly adopts a membrane filtration method, and the power consumption of a filtration membrane is 294kW & h per hour, so that the method reduces the power consumption by 63%.
The traditional method needs 180m in production3Fermentation broth and 135m3The temperature of the water is raised from 30 ℃ to 70 ℃, and the temperature is required to be 50 ℃ and the volume is 150m3The temperature of the 3 neutralizing tanks is raised to 90 ℃, and 0.5MPa saturated steam is consumed for about 46T. The method can extract the dibasic acid from the fermentation liquor at normal temperature without heating, and does not need steam in other steps except the drying step.
In equipment maintenance, filtration membrane equipment in the traditional production method needs to be supported by an automatic control system, most filtration membrane equipment is imported equipment, maintenance cost is high, and high-grade professionals are required to maintain under special conditions, so that the cost is high. The method adopts the domestic horizontal spiral centrifuge to complete the separation of the long-chain dicarboxylic acid and the thalli, and the domestic horizontal spiral centrifuge does not need a professional automatic control system, so that the maintenance cost is lower and the method is more reliable.
The membrane filtration system in the traditional production method is imported professional equipment, the operation of the equipment needs a lot of time training before operators are on duty, the requirements on the academic history and the quality of the operators are high, and misoperation is easy to occur in the production process, so that danger and loss are caused. The horizontal spiral centrifuge used in the method is simple to operate, professional long-term training is not needed before operators are on duty, personnel training cost and period are reduced, labor cost is reduced, errors are not prone to occurring in the operation of the method, and dangers and losses occurring in production are reduced.
Comparative example 2 (drum centrifuge):
in the extraction apparatus of the present invention, it was found that, in an experiment using a drum centrifuge instead of a horizontal screw centrifuge, since the former has a filter type operation principle and the latter has a screw decanter type operation principle, when the former separates a dibasic acid from cells, a solid layer formed by the accumulation of a dibasic acid solid on a drum causes a filter effect on the cells, which further prevents the cells from being filtered, and the separation effect of the dibasic acid from the cells cannot be achieved.
Therefore, the method has the beneficial effects that the centrifugation method of the domestic horizontal spiral centrifuge is adopted to replace the membrane filtration method of an imported filtration membrane to separate the impurities such as the long-chain dicarboxylic acid, the thalli and the like from the fermentation liquor, the equipment investment can be reduced, the consumption of water, electricity and steam can be reduced under the condition of ensuring the production efficiency and the product quality, a cleaning agent is not required, and the reliability is higher.
The method for extracting the long-chain dicarboxylic acid from the fermentation liquor provided by the invention has the advantages that hazardous chemicals such as strong acid, strong base and the like are not used in all processes, the fermentation liquor is not required to be heated, the production can be completed under the conditions that the pH value of the fermentation liquor is 6.5-7.5 and the temperature is 28-30 ℃, the use of the hazardous chemicals such as the strong acid, the strong base and the like can be reduced, the discharge amount of waste water and the content of sodium sulfate in the waste water are reduced, further, the application environment for separating the long-chain dicarboxylic acid from thalli can reduce the consumption of water, electricity and steam, the equipment investment is less, the industrial amplification production is facilitated, the waste water treatment cost is lower, and the production is more environment-friendly.
Claims (10)
1. A method for extracting long-chain dicarboxylic acid from fermentation liquor comprises the following steps:
s1: inputting the fermented liquid into a fermented liquid storage tank after fermentation;
s2: primary centrifugation: conveying the fermentation liquor into a first horizontal spiral centrifuge by a fermentation liquor storage tank to obtain a long-chain dibasic acid solid phase and a liquid phase mainly containing thalli, inputting the long-chain dibasic acid solid phase into a first slurry mixing tank, and inputting the liquid phase mainly containing thalli into a mother liquor tank;
s3: primary water adding and size mixing: adding normal-temperature softened water into the first slurry mixing tank, starting the first slurry mixing tank to stir after the long-chain dicarboxylic acid solid phase enters the first slurry mixing tank, and forming a long-chain dicarboxylic acid solid-liquid mixed material;
s4: and (3) secondary centrifugation: conveying the long-chain dicarboxylic acid solid-liquid mixed material in the first slurry mixing tank into a second horizontal spiral centrifugal machine to obtain a long-chain dicarboxylic acid solid phase and a liquid phase containing a small amount of thalli, and conveying the liquid phase containing the small amount of thalli into a mother liquor tank;
s5: and (3) secondary water adding and size mixing: conveying the long-chain dicarboxylic acid solid phase to a second slurry mixing tank by a second horizontal spiral centrifuge, adding normal-temperature softened water into the second slurry mixing tank, and opening the second slurry mixing tank to stir after the long-chain dicarboxylic acid solid phase enters the second slurry mixing tank to form a long-chain dicarboxylic acid solid-liquid mixed material;
s6: and (3) filter pressing: and conveying the long-chain dicarboxylic acid solid-liquid mixed material in the second slurry mixing tank into a plate-and-frame filter press, cleaning, squeezing and blow-drying to obtain a long-chain dicarboxylic acid solid phase.
2. The method of claim 1, wherein the step of extracting the long-chain dicarboxylic acid from the fermentation broth comprises: further comprising step S7: and (3) drying: and conveying the long-chain dicarboxylic acid solid phase subjected to filter pressing into a flash evaporation dryer through a screw conveyor, and drying to obtain a long-chain dicarboxylic acid finished product with the purity of more than 97% and the moisture of less than 0.3%.
3. The method of claim 1, wherein the step of extracting the long-chain dicarboxylic acid from the fermentation broth comprises: in step S1, the pH of the fermentation liquid is 6.5-7.5, and the temperature is 28-30 ℃.
4. The method of claim 1, wherein the step of extracting the long-chain dicarboxylic acid from the fermentation broth comprises: the rotating speed of the first horizontal spiral centrifugal machine in the step S2 is 1000r/min-1300r/min during operation; and the rotating speed of the second horizontal spiral centrifugal machine in the step S4 is 2000r/min-5000r/min during operation.
5. The method of claim 1, wherein the step of extracting the long-chain dicarboxylic acid from the fermentation broth comprises: in step S3, the ratio of the water content to the solid phase in the long-chain dicarboxylic acid solid-liquid mixed material is 1:1-2: 1.
6. The method of claim 1, wherein the step of extracting the long-chain dicarboxylic acid from the fermentation broth comprises: in step S4, sampling and inspecting the long-chain dibasic acid solid phase output by the second horizontal type spiral centrifugal machine, directly conveying the long-chain dibasic acid solid phase to a spiral conveyer when the total nitrogen content of the long-chain dibasic acid solid phase is not more than 0.01%, and performing drying treatment in step S7; and when the total nitrogen content of the long-chain dibasic acid solid phase is higher than 0.01%, conveying the long-chain dibasic acid solid phase to a second slurry mixing tank, and continuing to process in the following step S5.
7. The method of claim 1, wherein the step of extracting the long-chain dicarboxylic acid from the fermentation broth comprises: in step S5, the ratio of water to solid phase in the long-chain dicarboxylic acid solid-liquid mixed material is 1:1-2: 1.
8. The method of claim 6, wherein the step of extracting the long-chain dicarboxylic acid from the fermentation broth comprises: the secondary centrifugation of step S4 and the secondary water-adding slurry mixing of step S5 can be reused several times before step S6 as a combination for removing impurities.
9. The method of claim 7, wherein the step of extracting the long-chain dicarboxylic acid from the fermentation broth comprises: the ratio of water to solid phase in the long-chain dicarboxylic acid solid-liquid mixed material is 1.5: 1.
10. The product produced by the method for extracting long-chain dicarboxylic acid from fermentation broth according to any one of claims 1 to 9, wherein: the product comprises one or more of C10-C18 long-chain dibasic acids.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103570525A (en) * | 2012-07-25 | 2014-02-12 | 中国石油化工股份有限公司 | Method for refining long-chain dibasic acid |
| CN110218746A (en) * | 2018-03-01 | 2019-09-10 | 上海凯赛生物技术研发中心有限公司 | The method and fermentation liquid of fermenting and producing long-chain biatomic acid, fermentation treatment fluid, sewage |
| CN211445571U (en) * | 2019-12-31 | 2020-09-08 | 凯赛（金乡）生物材料有限公司 | System for producing long-chain dicarboxylic acid by utilizing biological fermentation method |
| CN113461514A (en) * | 2020-03-31 | 2021-10-01 | 上海凯赛生物技术股份有限公司 | Method for extracting long-chain dicarboxylic acid from fermentation liquor |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103570525A (en) * | 2012-07-25 | 2014-02-12 | 中国石油化工股份有限公司 | Method for refining long-chain dibasic acid |
| CN110218746A (en) * | 2018-03-01 | 2019-09-10 | 上海凯赛生物技术研发中心有限公司 | The method and fermentation liquid of fermenting and producing long-chain biatomic acid, fermentation treatment fluid, sewage |
| CN211445571U (en) * | 2019-12-31 | 2020-09-08 | 凯赛（金乡）生物材料有限公司 | System for producing long-chain dicarboxylic acid by utilizing biological fermentation method |
| CN113461514A (en) * | 2020-03-31 | 2021-10-01 | 上海凯赛生物技术股份有限公司 | Method for extracting long-chain dicarboxylic acid from fermentation liquor |
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