Extraction and concentration device for 1, 3-propylene glycol fermentation liquor

Abstract

The utility model discloses an extraction and concentration device for 1, 3-propylene glycol fermentation liquor, which is characterized in that an alcohol diluting tank is used for diluting the 1, 3-propylene glycol fermentation liquor; the centrifugal precipitation device is connected to the alcohol diluting tank and is used for receiving the alcohol-diluted 1, 3-propylene glycol fermentation liquor from the alcohol diluting tank and carrying out centrifugal precipitation removal; the storage tank is connected to the centrifugal precipitation device and is used for receiving supernate from the centrifugal precipitation device; the ultrafiltration membrane system is connected to the storage tank and is used for performing ultrafiltration on the supernate; the purification device is connected to the permeation side of the ultrafiltration membrane system and is used for purifying filtrate of the ultrafiltration membrane system; the membrane concentration system is connected to an eluent outlet of the purification device and is used for concentrating and dehydrating the purified and desorbed feed liquid; and the dehydrating tower is connected to the concentrated solution side of the membrane concentration system, is sequentially connected with the dealcoholization tower and the light component removal tower, and is used for separating deionized water, n-butyl alcohol and residual light components with boiling points lower than that of 1, 3-propylene glycol in the fermentation liquor to obtain high-purity 1, 3-propylene glycol.

Description

Technical Field

[0001] The utility model relates to an extraction and concentration device for 1,3-propylene glycol fermentation liquid, belonging to the technical field of biological fermentation purification. Background Art

[0002] 1,3-propylene glycol is an important chemical raw material, mainly used to synthesize new polyester materials such as polytrimethylene terephthalate, polyurethane and engineering thermoplastics. Compared with chemical synthesis, the production of 1,3-propylene glycol by microbial fermentation has significant advantages: 1. It can use low-cost renewable resources (such as corn and starch) as raw materials; 2. The production conditions are mild, generally operated at room temperature, and no precious metal catalysts are required; 3. It has good selectivity and few by-products; 4. It has no environmental pollution. Microbial fermentation is a "green industry" characterized by biotechnology, and therefore it is increasingly valued.

[0003] The concentration of 1,3-propylene glycol in the fermentation broth produced by the microbial fermentation method is low, and the fermentation broth is complex, including bacteria, proteins, and suspended matter. For 1,3-propylene glycol fermentation broth, due to the strong hydrophilicity of 1,3-propylene glycol, ordinary methods are not suitable for this system, making its separation difficult and the product purity low. Therefore, it is urgent to provide an extraction and concentration device for 1,3-propylene glycol fermentation broth that can improve the purity of the product. Utility Model Content

[0004] The utility model aims to provide an extraction and concentration device for 1,3-propylene glycol fermentation broth, which can effectively improve the purity of the product.

[0005] In order to achieve the above purpose, the technical solution adopted by the utility model is:

[0006] A device for extracting and concentrating 1,3-propylene glycol fermentation broth, comprising:

[0007] Alcohol dilution tank, used for diluting 1,3-propylene glycol fermentation broth;

[0008] A centrifugal sedimentation device is connected to the alcohol dilution tank and is used to receive the 1,3-propylene glycol fermentation liquid after alcohol dilution in the alcohol dilution tank and perform centrifugal sedimentation;

[0009] a storage tank connected to the centrifugal sedimentation device and used to receive the supernatant from the centrifugal sedimentation device;

[0010] An ultrafiltration membrane system, connected to the storage tank, for ultrafiltration of the supernatant;

[0011] A purification device, connected to the permeation side of the ultrafiltration membrane system, for purifying the filtrate of the ultrafiltration membrane system;

[0012] The membrane concentration system is connected to the eluent outlet of the purification device and is used to concentrate and dehydrate the purified liquid after adsorption;

[0013] A dehydration tower, connected to the concentrated liquid side of the membrane concentration system, is used to dehydrate the concentrated liquid;

[0014] A dealcoholization tower connected to the liquid outlet of the dehydration tower is used to dealcoholize the dehydrated liquid;

[0015] The light-removal tower is connected to the liquid outlet of the dealcoholization tower and is used to remove light components from the liquid after dealcoholization to obtain 1,3-propylene glycol.

[0016] Preferably, the membrane in the ultrafiltration membrane system is a ceramic membrane with multiple channels.

[0017] Preferably, the molecular weight cut-off of the ceramic membrane is 1-30KD.

[0018] Preferably, the purification device is an ion exchange resin column.

[0019] Preferably, the membrane in the membrane concentration system is a reverse osmosis membrane.

[0020] Preferably, the molecular weight cut-off of the reverse osmosis membrane is 50-400Da.

[0021] Preferably, the permeate outlet of the membrane concentration system is connected to the liquid inlet of the ultrafiltration membrane system.

[0022] Preferably, a filter is also installed on the pipeline between the alcohol dilution tank and the centrifugal sedimentation device.

[0023] The beneficial effects of the utility model are:

[0024] The method utilizes the alcohol precipitation effect of n-butanol on the protein in the fermentation broth to make it cluster, which is then beneficial for subsequent centrifugal precipitation; then a centrifugal precipitation device, an ultrafiltration membrane system, and a purification device are used in sequence to remove impurities such as bacteria, suspended matter, protein, small molecule polypeptides, and pigments in the fermentation broth to improve the purity of the product; finally, a membrane concentration system, a dehydration tower, a dealcoholization tower, and a lightness removal tower are used to separate deionized water (boiling point 100°C), n-butanol (boiling point 117-118°C), and residual light components with a boiling point lower than 1,3-propylene glycol (210-211°C) in the fermentation broth to further improve the purity of the product; at the same time, the permeate of the membrane concentration system is reused as dialysis water of the ultrafiltration membrane system, which can improve the product yield to a certain extent. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 This is the flow chart of this patent;

[0026] Figure 2This is a device diagram of this patent.

[0027] The main reference numerals in the figure have the following meanings:

[0028] 1. Alcohol dilution tank, 2. Filter, 3. Centrifugal sedimentation device, 4. Storage tank, 5. Ultrafiltration membrane system, 6. Purification device, 7. Membrane concentration system, 8. Dehydration tower, 9. Dealcoholization tower, 10. Lightness removal tower, 11. Pump. DETAILED DESCRIPTION

[0029] The utility model is specifically introduced below in conjunction with the accompanying drawings and embodiments.

[0030] like Figure 1-2 As shown, the utility model is an extraction and concentration device for 1,3-propylene glycol fermentation broth, comprising an alcohol dilution tank 1, a filter 2, a machine pump 11 (boosting pump or centrifugal pump, the same below), a centrifugal sedimentation device 3, a storage tank 4, a machine pump 11, an ultrafiltration membrane system 5, a purification device 6, a membrane concentration system 7, a dehydration tower 8, a machine pump 11, a dealcoholization tower 9, a machine pump 11, a lightness removal tower 10 and a machine pump 11, which are sequentially connected through pipelines, and the permeate outlet of the membrane concentration system 7 is connected to the liquid inlet of the ultrafiltration membrane system 5.

[0031] The alcohol dilution tank 1 is used for alcohol dilution of 1,3-propylene glycol fermentation broth. n-Butanol and 1,3-propylene glycol fermentation broth are added to the alcohol dilution tank 1 and mixed evenly. The mixed liquid is then pumped to the centrifugal sedimentation device 3 by the pump 11 for centrifugal precipitation treatment. The supernatant overflows into the storage tank 4. The liquid collected in the storage tank 4 is then pumped to the ultrafiltration membrane system 5 by the pump 11. The ultrafiltration membrane is used to remove residual bacteria, suspended matter, large molecular proteins and other impurities to obtain an ultrafiltration clear liquid with extremely low protein content. The ultrafiltration clear liquid enters the purification device 6 to further remove small molecular polypeptides and pigments. The chromatographic separation and purification liquid of 1,3-propylene glycol with high purity is then obtained after analysis; the chromatographic separation and purification liquid is then passed through a membrane concentration system 7 to remove part of the water to obtain a 1,3-propylene glycol concentrate and deionized water, and the deionized water is reused as the dialysis water of the ultrafiltration membrane system 5 to improve the yield of 1,3-propylene glycol; the 1,3-propylene glycol concentrate is then passed through a dehydration tower 8, a dealcoholization tower 9 and a light component removal tower 10 in sequence to separate the deionized water, n-butanol and residual light components with a boiling point lower than that of 1,3-propylene glycol in the concentration to obtain high-purity 1,3-propylene glycol.

[0032] Furthermore, the membrane in the ultrafiltration membrane system 5 is a low molecular weight ceramic membrane, the molecular weight cut-off of the ceramic membrane is 1-30KD, preferably 15KD, the ceramic membrane has a diameter of 52mm, a length of 1.5m, 61 channels with a channel diameter of 4mm, and a single membrane tube filtration area of ​​1.29m 2In the ultrafiltration membrane system 5, the system operating pressure is 0.6-1 MPa, the membrane surface flow rate is 4 m / s, and the concentration multiple is 20-30 times. The purification device 6 is an ion exchange resin column. The membrane in the membrane concentration system 7 is a reverse osmosis membrane with a molecular weight cutoff of 50-400 Da.

[0033] Furthermore, the precipitate in the centrifugal sedimentation device 3 is collected and the resulting solution can be reused in the alcohol dilution tank 1; the deionized water and n-butanol evaporated from the dehydration tower 8 and the dealcoholization tower 9 can be recovered and reused.

[0034] Example 1

[0035] In step 1, n-butanol and 1,3-propylene glycol fermentation broth are added into the alcohol dilution tank 1 and mixed evenly, and then the mixed liquid is pumped into the centrifugal sedimentation device 3 for centrifugal sedimentation treatment, and the supernatant of the centrifugal sedimentation device 3 overflows into the storage tank 4.

[0036] Step 2: Pump the feed liquid in the storage tank 4 to the ultrafiltration membrane system 5 to remove impurities such as residual bacteria, suspended matter and macromolecular proteins to obtain ultrafiltration clear liquid with extremely low protein content;

[0037] Among them, the operating pressure of ultrafiltration membrane system 5 is 0.6MPa, the membrane surface flow rate is 4m / s, and the concentration multiple is 20 times; the membrane used is a ceramic membrane with a corresponding molecular weight cutoff of 15KD. The ceramic membrane has a diameter of 52mm and a length of 1.5m. It has 61 channels with a channel diameter of 4mm. The filtration area of ​​a single membrane tube is 1.29m 2 .

[0038] Step 3: The ultrafiltration clear liquid enters the purification device 6, through which the effective ingredients are adsorbed and impurities such as small molecule peptides and pigments are further removed, and after analysis, a chromatographic separation purified liquid of 1,3-propylene glycol with high purity is obtained.

[0039] Step 4: The 1,3-propylene glycol chromatographic separation and purification liquid passes through a membrane concentration system 7, and a reverse osmosis membrane is used to concentrate the 1,3-propylene glycol chromatographic separation and purification liquid to remove part of the water, thereby obtaining a 1,3-propylene glycol concentrate and deionized water, and the deionized water is reused as dialysis water of an ultrafiltration membrane system 5;

[0040] Among them, the filter element in the membrane concentration system 7 has a corresponding molecular weight cutoff of 100Da, and the system operating pressure is 2MPa.

[0041] In step 5, the 1,3-propylene glycol concentrate is sequentially passed through a dehydration tower 8, a dealcoholization tower 9, and a light component removal tower 10 to distill off deionized water (boiling point 100° C.), n-butanol (boiling point 117-118° C.) and residual light components with a boiling point lower than that of 1,3-propylene glycol (210-211° C.) in the 1,3-propylene glycol concentrate to obtain 1,3-propylene glycol.

[0042] Comparative Example 1

[0043] The difference from Example 1 is that the water removed by the membrane concentration system 7 is not reused.

[0044] In step 1, n-butanol and 1,3-propylene glycol fermentation broth are added into the alcohol dilution tank 1 and mixed evenly, and then the mixed liquid is pumped into the centrifugal sedimentation device 3 for centrifugal sedimentation treatment, and the supernatant of the centrifugal sedimentation device 3 overflows into the storage tank 4.

[0045] Step 2: Pump the feed liquid in the storage tank 4 to the ultrafiltration membrane system 5 to remove impurities such as residual bacteria, suspended matter and macromolecular proteins to obtain ultrafiltration clear liquid with extremely low protein content;

[0046] Among them, the operating pressure of ultrafiltration membrane system 5 is 0.6MPa, the membrane surface flow rate is 4m / s, and the concentration multiple is 20 times; the membrane used is a ceramic membrane with a corresponding molecular weight cutoff of 15KD. The ceramic membrane has a diameter of 52mm and a length of 1.5m. It has 61 channels with a channel diameter of 4mm. The filtration area of ​​a single membrane tube is 1.29m 2 .

[0047] Step 3: The ultrafiltration clear liquid enters the purification device 6, through which the effective ingredients are adsorbed and impurities such as small molecule peptides and pigments are further removed, and after analysis, a chromatographic separation purified liquid of 1,3-propylene glycol with high purity is obtained.

[0048] Step 4, the 1,3-propylene glycol chromatographic separation and purification liquid passes through a membrane concentration system 7, and a reverse osmosis membrane is used to concentrate the 1,3-propylene glycol chromatographic separation and purification liquid to remove part of the water, thereby obtaining a 1,3-propylene glycol concentrate and deionized water;

[0049] Among them, the filter element in the membrane concentration system 7 has a corresponding molecular weight cutoff of 100Da, and the system operating pressure is 2MPa.

[0050] In step 5, the 1,3-propylene glycol concentrate is sequentially passed through a dehydration tower 8, a dealcoholization tower 9, and a light component removal tower 10 to distill off deionized water (boiling point 100° C.), n-butanol (boiling point 117-118° C.) and residual light components with a boiling point lower than that of 1,3-propylene glycol (210-211° C.) in the 1,3-propylene glycol concentrate to obtain 1,3-propylene glycol.

[0051] Comparative Example 2

[0052] The difference from Example 1 is that the centrifugal sedimentation device 3 is not used to remove part of the impurities first.

[0053] Step 1: adding n-butanol and 1,3-propylene glycol fermentation broth into an alcohol dilution tank 1 and mixing them evenly, and then pumping the mixed liquid to an ultrafiltration membrane system 5 to remove impurities such as bacteria, suspended matter, and macromolecular proteins to obtain a filtrate;

[0054] Among them, the operating pressure of ultrafiltration membrane system 5 is 0.6MPa, the membrane surface flow rate is 4m / s, and the concentration multiple is 20 times; the membrane used is a ceramic membrane with a corresponding molecular weight cutoff of 15KD. The ceramic membrane has a diameter of 52mm and a length of 1.5m. It has 61 channels with a channel diameter of 4mm. The filtration area of ​​a single membrane tube is 1.29m 2 .

[0055] In step 2, the filtrate enters the purification device 6, through which the effective ingredients are adsorbed and impurities such as small molecule peptides and pigments are further removed, and after analysis, 1,3-propylene glycol chromatographic separation purified liquid is obtained.

[0056] Step 3, the 1,3-propylene glycol chromatographic separation and purification liquid passes through a membrane concentration system 7, and a reverse osmosis membrane is used to concentrate the 1,3-propylene glycol chromatographic separation and purification liquid to remove part of the water, thereby obtaining a 1,3-propylene glycol concentrate and deionized water;

[0057] Among them, the filter element in the membrane concentration system 7 has a corresponding molecular weight cutoff of 100Da, and the system operating pressure is 2MPa.

[0058] In step 4, the 1,3-propylene glycol concentrate is sequentially passed through a dehydration tower 8, a dealcoholization tower 9, and a light component removal tower 10 to distill off deionized water (boiling point 100° C.), n-butanol (boiling point 117-118° C.) and residual light components with a boiling point lower than that of 1,3-propylene glycol (210-211° C.) in the 1,3-propylene glycol concentrate to obtain 1,3-propylene glycol.

[0059] The yield of 1,3-propylene glycol obtained in Example 1 and Comparative Examples 1-2 was calculated and the purity of the product was tested. The results are shown in Table 1.

[0060] Table 1 Yield and purity of 1,3-propylene glycol obtained in Example 1 and Comparative Examples 1-2

[0061] 1,3-Propanediol yield 1,3-Propanediol Purity Example 1 95-97％ 98.3-99.5％ Comparative Example 1 93-95％ 97.6-99.1％ Comparative Example 2 94-96％ 94.3-95.5％

[0062] It can be seen from Table 1 that after the 1,3-propylene glycol fermentation broth is treated by the extraction and concentration device provided by the utility model, the yield and purity of 1,3-propylene glycol can be improved to a certain extent.

[0063] The above is only a preferred implementation of the utility model patent. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the utility model patent. These improvements and modifications should also be regarded as the protection scope of the utility model patent.

Claims

1. A device for extracting and concentrating 1,3-propylene glycol fermentation broth, characterized in that: include: Alcohol dilution tank, used for diluting 1,3-propylene glycol fermentation broth; A centrifugal sedimentation device is connected to the alcohol dilution tank and is used to receive the 1,3-propylene glycol fermentation liquid after alcohol dilution in the alcohol dilution tank and perform centrifugal sedimentation; a storage tank connected to the centrifugal sedimentation device and used to receive the supernatant from the centrifugal sedimentation device; An ultrafiltration membrane system, connected to the storage tank, for ultrafiltration of the supernatant; A purification device, connected to the permeation side of the ultrafiltration membrane system, for purifying the filtrate of the ultrafiltration membrane system; The membrane concentration system is connected to the eluent outlet of the purification device and is used to concentrate and dehydrate the purified liquid after adsorption; A dehydration tower, connected to the concentrated liquid side of the membrane concentration system, is used to dehydrate the concentrated liquid; A dealcoholization tower, connected to the liquid outlet of the dehydration tower, for dealcoholizing the dehydrated liquid; The light-removal tower is connected to the liquid outlet of the dealcoholization tower and is used to remove light components from the liquid after dealcoholization to obtain 1,3-propylene glycol.

2. The extraction and concentration device for 1,3-propylene glycol fermentation broth according to claim 1, characterized in that: The membrane in the ultrafiltration membrane system is a ceramic membrane with multiple channels.

3. The extraction and concentration device for 1,3-propylene glycol fermentation broth according to claim 2, characterized in that: The molecular weight cut-off of the ceramic membrane is 1-30KD.

4. The extraction and concentration device for 1,3-propylene glycol fermentation broth according to claim 1, characterized in that: The purification device is an ion exchange resin column.

5. The extraction and concentration device for 1,3-propylene glycol fermentation broth according to claim 1, characterized in that: The membrane in the membrane concentration system is a reverse osmosis membrane.

6. The extraction and concentration device for 1,3-propylene glycol fermentation broth according to claim 5, characterized in that: The molecular weight cut-off of the reverse osmosis membrane is 50-400Da.

7. The extraction and concentration device for 1,3-propylene glycol fermentation broth according to claim 1, 5 or 6, characterized in that: The permeate outlet of the membrane concentration system is connected to the liquid inlet of the ultrafiltration membrane system.

8. The extraction and concentration device for 1,3-propylene glycol fermentation broth according to claim 1, characterized in that: A filter is also installed on the pipeline between the alcohol dilution tank and the centrifugal sedimentation device.

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