CN214299947U - 1, 5-pentanediamine extraction system - Google Patents
1, 5-pentanediamine extraction system Download PDFInfo
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- CN214299947U CN214299947U CN202022228743.8U CN202022228743U CN214299947U CN 214299947 U CN214299947 U CN 214299947U CN 202022228743 U CN202022228743 U CN 202022228743U CN 214299947 U CN214299947 U CN 214299947U
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Abstract
The utility model provides an extraction system of 1, 5-pentanediamine for extract 1, 5-pentanediamine from first mixture, first mixture includes 1, 5-pentanediamine salt, metal ion and water, extraction system includes adsorption unit, electrodialysis unit and extraction element; the adsorption unit is used for adsorbing the metal ions in the first mixture to obtain a second mixture; the electrodialysis unit is used for carrying out electrodialysis treatment on the second mixture to obtain an aqueous solution containing 1, 5-pentanediamine; the extraction unit is used for separating 1, 5-pentanediamine from the aqueous solution containing the 1, 5-pentanediamine; wherein the adsorption unit is provided with resin, and the electrodialysis unit is provided with a bipolar membrane electrodialysis device. The utility model discloses an extraction system of embodiment can effectively get rid of the impurity in the first mixture, and the purity of the 1, 5-pentanediamine product of gained is high, the yield is high.
Description
Technical Field
The utility model relates to an extract the purification device, specifically be a system for draw 1, 5-pentanediamine from 1, 5-pentanediamine salt solution.
Background
1, 5-Pentanediamine (Diaminopentane; DN5, hereinafter pentanediamine), also known as cadaverine. Solutions containing 1, 5-pentanediamine salt are generally obtained industrially by fermentation or enzymatic conversion processes. At the end of the fermentation or enzymatic conversion, the pH of the fermentation broth or enzymatic conversion broth is generally close to neutral and the pentanediamine is present in the aqueous solution in the form of a salt (e.g., pentanediamine sulfate, pentanediamine carbonate, pentanediamine hydrochloride, etc.). Further extracting and purifying the salt solution of the 1, 5-pentanediamine to obtain the 1, 5-pentanediamine.
The pentanediamine can replace hexamethylenediamine to produce nylon 5X (such as nylon 54, nylon 56 and the like) by polymerization with dibasic acid, and the main application fields are fibers and engineering plastics. The total demand for global nylon exceeds 700 million tons/year, with the market demand for nylon 6X produced from hexamethylenediamine as a feedstock exceeding 200 million tons/year. The biological method for producing the pentanediamine can replace the imported hexanediamine, reduce the cost of raw materials, is beneficial to digesting the domestic surplus lysine productivity, prolongs the industrial value chain, forms the upstream-downstream linkage and has important social benefit and economic value.
At present, the main method for extracting and purifying pentamethylene diamine from biological fermentation liquor or enzyme conversion liquor is to add alkali into the fermentation liquor or enzyme conversion liquor containing pentamethylene diamine salt to produce pentamethylene diamine and salt (sulfate, carbonate, hydrochloride, etc.), and then obtain pentamethylene diamine through the treatment of a filter device, an extraction device or a distillation device. The method needs to consume a large amount of alkali, forms a large amount of solid slag and high-salt-content wastewater, and has high production cost and high environmental protection pressure. Therefore, there is a need to develop a method and a device for purifying pentamethylene diamine, which are environmentally friendly, safe, efficient and low in cost.
SUMMERY OF THE UTILITY MODEL
In order to solve the technical problem, the utility model provides an extraction system of 1, 5-pentanediamine, be used for extracting 1, 5-pentanediamine from first mixture, first mixture includes 1, 5-pentanediamine salt, metal ion and water, extraction system includes adsorption unit, electrodialysis unit and extraction element; the adsorption unit is used for adsorbing the metal ions in the first mixture to obtain a second mixture; the electrodialysis unit is used for carrying out electrodialysis treatment on the second mixture to obtain an aqueous solution containing 1, 5-pentanediamine; the extraction unit is used for separating 1, 5-pentanediamine from the aqueous solution containing the 1, 5-pentanediamine; wherein the adsorption unit is provided with resin, and the electrodialysis unit is provided with a bipolar membrane electrodialysis device.
According to the utility model discloses an embodiment, extraction system includes the solid-liquid separation unit, set up in the upper reaches of absorption unit, it is right to be used for first mixture carries out solid-liquid separation and handles.
According to an embodiment of the present invention, a centrifuge and/or a membrane filtration device is provided in the solid-liquid separation unit, and a microfiltration membrane and/or an ultrafiltration membrane is provided in the membrane filtration device.
According to an embodiment of the present invention, the bipolar membrane electrodialysis device includes a first bipolar membrane, a second bipolar membrane, a cation exchange membrane and an anion exchange membrane, the cation exchange membrane the anion exchange membrane is located between the first bipolar membrane and the second bipolar membrane the cation exchange membrane with an alkali chamber is formed between the first bipolar membrane the anion exchange membrane with an acid chamber is formed between the second bipolar membrane the cation exchange membrane with a salt chamber is formed between the anion exchange membrane.
According to an embodiment of the present invention, the electrodialysis unit further comprises a concentration device for concentrating the second mixture remaining in the salt compartment.
According to an embodiment of the present invention, the concentration device is selected from an evaporative concentration device and/or an electrodialysis concentration device.
According to the utility model discloses an embodiment, the electrodialysis unit still includes first adsorption equipment, electrodialysis enrichment facility is including desalination room and concentration room, first adsorption equipment with the desalination room links to each other.
According to an embodiment of the present invention, the extraction unit comprises a distillation apparatus.
According to an embodiment of the present invention, the extraction unit further comprises a rectifying tower for further purifying the 1, 5-pentanediamine product separated by the distillation apparatus.
The utility model discloses an extraction system of embodiment can effectively get rid of the impurity in the first mixture, and the purity of the 1, 5-pentanediamine product of gained is high, the yield is high.
Drawings
The various objects, features and advantages of the present invention will become more apparent from the following detailed description of the preferred embodiments of the invention, when considered in conjunction with the accompanying drawings. The drawings are merely exemplary of the invention and are not necessarily drawn to scale.
FIG. 1 is a schematic structural diagram of an extraction system for 1, 5-pentanediamine according to an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of an extraction system for 1, 5-pentanediamine according to another embodiment of the present invention;
FIG. 3 is a schematic structural diagram of an extraction system for 1, 5-pentanediamine according to another embodiment of the present invention;
fig. 4 is a schematic structural view of a bipolar membrane electrodialysis device according to an embodiment of the present invention;
fig. 5 is a schematic structural diagram of an electrodialysis concentration device according to an embodiment of the present invention.
Wherein the reference numerals are as follows:
1a, a bipolar membrane; 1b, bipolar membrane; 2. a cation exchange membrane; 3. an anion exchange membrane; 4. a cathode; 5. an anode; 6. an alkali chamber; 7. a salt chamber; 8. an acid chamber; 11a, an anion exchange membrane; 11b, an anion exchange membrane; 12a, a cation exchange membrane; 12b, a cation exchange membrane; 13. a cathode; 14. and an anode.
Detailed Description
Exemplary embodiments that embody features and advantages of the invention are described in detail below. It is to be understood that the invention is capable of other and different embodiments and its several details are capable of modification without departing from the scope of the invention, and that the description and drawings are to be regarded as illustrative in nature and not as restrictive.
Referring to fig. 1 to 5, an embodiment of the present invention provides an extraction system of 1, 5-pentanediamine for extracting 1, 5-pentanediamine from a first mixture, the first mixture including 1, 5-pentanediamine salt, metal ions and water, the extraction system including:
the adsorption unit is used for removing metal ions in the first mixture to obtain a second mixture;
an electrodialysis unit, which is used for carrying out electrodialysis treatment on the second mixture to obtain an aqueous solution containing 1, 5-pentanediamine; and
an extraction unit for recovering 1, 5-pentanediamine from an aqueous solution containing 1, 5-pentanediamine;
wherein, resin is arranged in the adsorption unit, and the electrodialysis unit is provided with a bipolar membrane electrodialysis device.
In one embodiment, the metal ions include divalent metal ions, trivalent metal ions, and further include any one or a combination of two or more of calcium ions, magnesium ions, iron ions, zinc ions, copper ions, aluminum ions, and silicon ions.
In one embodiment, the second mixture comprises 1, 5-pentanediamine salt and water.
In one embodiment, the second mixture includes 1, 5-pentanediamine salt, water, and metal ions in an amount of 15ppm or less.
In one embodiment, the first mixture further comprises a pigment and a bacterial cell.
In one embodiment, the 1, 5-pentanediamine salt includes one, two, three, four or more of sulfate of 1, 5-pentanediamine, hydrochloride of 1, 5-pentanediamine, carbonate of 1, 5-pentanediamine, and phosphate of 1, 5-pentanediamine.
In the present invention, the concentration of the 1, 5-pentanediamine means the concentration of the 1, 5-pentanediamine converted from various forms of the 1, 5-pentanediamine (for example, the 1, 5-pentanediamine salt form, the 1, 5-pentanediamine, and the 1, 5-pentanediamine ion form) present in the system to the 1, 5-pentanediamine, unless otherwise specified. That is, the "concentration of 1, 5-pentanediamine" means the concentration in terms of 1, 5-pentanediamine.
In one embodiment, the concentration of 1, 5-pentanediamine in the first mixture may be 5 wt% to 30 wt%, and further 5 wt% to 20 wt%.
In one embodiment, the pH of the first mixture is 6 to 10.
In one embodiment, the first mixture may be a 1, 5-pentanediamine salt enzyme conversion solution, a 1, 5-pentanediamine salt fermentation broth, or an aqueous solution of 1, 5-pentanediamine salt.
The utility model discloses to 1, 5-pentamethylene diamine salt enzyme conversion solution or the direct fermentation preparation 1, 5-pentamethylene diamine's of preparation concrete method do not have special restrictions, and ordinary skilled person in the art can decide to select specific raw materials according to prior art, confirms the technological parameter of concrete enzyme conversion process to obtain the solution that contains 1, 5-pentamethylene diamine salt.
In one embodiment, the first mixture is a 1, 5-pentanediaminehydrase conversion solution, which can be obtained by reacting a lysine salt solution under the action of Lysine Decarboxylase (LDC). Wherein, the lysine salt can be inorganic salt or organic salt of lysine, such as lysine hydrochloride and lysine sulfate.
In one embodiment, the first mixture is a 1, 5-pentanediamine salt fermentation broth, which can be obtained by: by means of gene technology, the expression of lysine decarboxylase is up-regulated or recombinant expressed in the strain capable of producing lysine, and the produced lysine can be synchronously converted into pentanediamine in the fermentation process, so that the fermentation liquor containing 1, 5-pentanediamine salt is directly obtained.
The utility model has no special requirements for recombinant bacteria, as long as 1, 5-pentanediamine can be obtained. For example, "construction of a genetically engineered bacterium for producing 1, 5-pentanediamin corynebacterium glutamicum by one-step method" (Tan et al, J. China bioengineering, 2010, 30 (8): 93-99) discloses a recombinant strain obtained by using a genome of Hafniaalvei (Hafniaalvei) as a template, performing PCR amplification to obtain a lysine decarboxylase gene ldc, and cloning a target gene fragment obtained by amplification to the corynebacterium glutamicum by using shuttle plasmids of Escherichia coli (Escherichia coli)/Corynebacterium glutamicum (Corynebacterium glutamicum) as a vector. For another example, PCT/CN2015/094121 discloses a direct fermentative production of 1, 5-pentanediamine.
In one embodiment, the adsorption unit, the electrodialysis unit, and the extraction unit may be connected in sequence.
In one embodiment, the first mixture comprises bacteria, for example, the first mixture is a 1, 5-pentamethylene diamine salt enzyme conversion solution or a 1, 5-pentamethylene diamine salt fermentation solution, and a solid-liquid separation unit may be disposed before or upstream of the adsorption unit, and the solid-liquid separation unit may be connected to the adsorption unit to remove the bacteria from the first mixture before the obtained material is sent to the adsorption unit for absorption of metal ions.
In one embodiment, the solid-liquid separation unit is provided with a solid-liquid separation device, such as a centrifugal device and/or a membrane filtration device. The centrifuge apparatus comprises a centrifuge.
In one embodiment, a microfiltration membrane and/or an ultrafiltration membrane is disposed in the membrane filtration device, the microfiltration membrane can be a ceramic membrane, the pore size can be 0.03um to 0.2um, further 0.05um to 0.1um, and the pressure difference between the two sides of the membrane is 0.5 bar to 5 bar; the cutoff molecular weight of the ultrafiltration membrane can be 800-10000 Da, further can be 1000-5000 Da, and further can be 2000-5000 Da. The temperature of the microfiltration membrane is 20-90 ℃, and further 25-70 ℃; the temperature of ultrafiltration membrane filtration is 25-60 ℃, and further 30-60 ℃.
In one embodiment, the solid-liquid separation unit comprises a centrifuge, a microfiltration membrane and an ultrafiltration membrane arranged in sequence; during operation, the first mixture is firstly processed by a centrifuge, then membrane filtration is carried out by a microfiltration membrane and an ultrafiltration membrane, and the filtrate processed by the ultrafiltration membrane enters a subsequent adsorption unit.
In one embodiment, the resin in the adsorption unit comprises cation exchange resin, further comprises styrene-divinylbenzene cation exchange resin and polypropylene copolymer cation exchange resin, and the total exchange capacity of the resin is more than or equal to 2.0meq/ml, further more than or equal to 5.0meq/ml, further more than or equal to 6.5 meq/ml.
In one embodiment, the feed rate of the first mixture in the adsorption unit is 0.5 to 10 BV/h. Further 2 to 10BV/h, further 2 to 5 BV/h.
In one embodiment, the metal ion content of the obtained second mixture can be made 50ppm or less, further 30ppm or less, further 15ppm or less, further 10ppm or less, further 5ppm or less, further still further 1ppm or less by the resin treatment.
In one embodiment, the second mixture is subjected to bipolar membrane electrodialysis in a bipolar membrane electrodialysis device.
In one embodiment, referring to fig. 4, the bipolar membrane electrodialysis device includes bipolar membranes 1a and 1b, a cation exchange membrane 2 and an anion exchange membrane 3, wherein the cation exchange membrane 2 and the anion exchange membrane 3 are located between the bipolar membranes 1a and 1b, an alkali compartment 6 is formed between the cation exchange membrane 2 and the anion exchange membrane of the bipolar membrane 1a, an acid compartment 8 is formed between the anion exchange membrane 3 and the cation exchange membrane of the bipolar membrane 1b, a salt compartment 7 is formed between the cation exchange membrane 2 and the anion exchange membrane 3, and an anode 5 and a cathode 4 are respectively located on the sides of the bipolar membranes 1a and 1b far away from the cation exchange membrane 2 and the anion exchange membrane 3.
In one embodiment, the bipolar membrane electrodialysis device comprises a salt compartment liquid storage tank connected with the salt compartment 7, an alkali compartment liquid storage tank connected with the alkali compartment 6, and an acid compartment liquid storage tank connected with the acid compartment 8; the salt chamber liquid storage tank is used for containing a raw material second mixture (1, 5-pentanediamine salt solution) for performing bipolar membrane electrodialysis treatment, the alkali chamber liquid storage tank is used for collecting alkali formed in the alkali chamber 6, and the acid chamber liquid storage tank is used for collecting acid formed in the acid chamber 8.
In one embodiment, the number of the salt chamber liquid storage tanks, the number of the alkali chamber liquid storage tanks, and the number of the acid chamber liquid storage tanks are two or more.
In one embodiment, in operation, the second mixture is passed into the salt compartment 7 of the bipolar membrane electrodialysis device, under the action of the electric field, 1, 5-pentanediamine ions pass through the cation exchange membrane 2 into the alkali compartment 6 and are blocked by the anion exchange membrane of the bipolar membrane 1a to stay in the alkali compartment 6, and acid anions (sulfate, carbonate, phosphate, chloride, etc.) pass through the anion exchange membrane 3 into the acid compartment 8 and are blocked by the cation exchange membrane of the bipolar membrane 1b to stay in the acid compartment 8; under the action of an electric field and an intermediate catalytic layer of the bipolar membrane, water is electrolyzed into hydrogen ions and hydroxide ions, the hydroxide ions penetrate through an anion exchange membrane of the bipolar membrane 1a to enter an alkali chamber 6 and are combined with 1, 5-pentanediamine ions to form 1, 5-pentanediamine, so that an aqueous solution of the 1, 5-pentanediamine is obtained, and the hydrogen ions penetrate through a cation exchange membrane of the bipolar membrane 1b to enter an acid chamber 8 and are combined with acid radical anions to form acid.
In one embodiment, the bipolar membrane electrodialysis device further comprises an electrode chamber, a cathode chamber and an anode chamber are respectively formed between the cathode and the anode and the electrode membrane, and an electrode solution is introduced into the cathode chamber and the anode chamber, wherein the electrode solution comprises a sulfuric acid solution and a sulfate solution, such as a sodium sulfate solution; the concentration of the polar liquid can be 2-5 wt%.
In one embodiment, during the bipolar membrane electrodialysis treatment, the second mixture is passed into the salt compartment 7 of the bipolar membrane electrodialysis device for treatment, when the conductivity of the solution in the base compartment 6 is higher than 4.2mS/cm or the 1, 5-pentanediamine concentration of the solution in the base compartment 6 is higher than 6 wt%, further higher than 10 wt%, the solution in the base compartment 6 is drained and the solution enters a salt compartment liquid storage tank connected to the base compartment 6, i.e. an aqueous solution containing 1, 5-pentanediamine. Meanwhile, the alkali chamber 6 is connected to the next alkali chamber liquid storage tank.
When the conductivity of the solution in the salt compartment 7 is below 22mS/cm, further below 18mS/cm, or the 1, 5-pentanediamine concentration is below 3 wt%, further below 1.5 wt%, the remaining second mixture (1, 5-pentanediamine salt solution) in the salt compartment liquid storage tank is discharged. In one embodiment, the 1, 5-pentanediamine solution discharged from the salt compartment is recovered. Concentrating by electrodialysis and/or distillation to recover 1, 5-pentanediamine.
When the conductivity of the solution in the acid chamber 8 is higher than 300mS/cm, further higher than 400mS/cm or the acid radical concentration is higher than 0.8mol/L, further higher than 1mol/L, the acid solution in the acid chamber liquid storage tank is discharged.
In one embodiment, in the bipolar membrane electrodialysis treatment process, the membrane pair voltage is 1-6V, and further 2-5V; the current density is 400-900A/m2(ii) a The temperature is 10-60 ℃, further 10-40 ℃, and further 30-40 ℃; the linear velocity of each membrane surface is 0.5-7 cm/s, and further 2-4 cm/s.
In one embodiment, the acid solution discharged from the acid chamber 8 can be used comprehensively.
In one embodiment, the electrodialysis unit comprises a concentration device, which may be connected to the salt compartment 7 of the bipolar membrane electrodialysis device. After the bipolar membrane electrodialysis treatment is finished, the residual 1, 5-pentanediamine salt solution in the salt chamber 7 can be sent to a concentration device for concentration treatment, and the obtained concentrated solution can be sent to the salt chamber 7 again for the bipolar membrane electrodialysis treatment.
In one embodiment, the concentration device may be an evaporative concentration device and/or an electrodialysis concentration device.
In one embodiment, as shown in fig. 5, the electrodialysis concentration device includes an anion exchange membrane 11a, an anion exchange membrane 11b, a cation exchange membrane 12a, a cation exchange membrane 12b, a cathode 13 and an anode 14, wherein the anion exchange membrane 11a, the cation exchange membrane 12a, the anion exchange membrane 11b and the cation exchange membrane 12b are sequentially arranged, concentration chambers 15a and 15b are respectively formed between the anion exchange membrane 11a and the cation exchange membrane 12a and between the anion exchange membrane 11b and the cation exchange membrane 12b, and a desalination chamber 16 is formed between the cation exchange membrane 12a and the anion exchange membrane 11 b.
During operation, 1, 5-pentanediamine salt solution to be concentrated (namely the residual 1, 5-pentanediamine salt solution in the salt chamber 7 of the bipolar membrane electrodialysis device) is introduced into the desalting chamber 16, under the action of an electric field, 1, 5-pentanediamine ions pass through the cation exchange membranes 12a and 12b to enter the concentrating chambers 15a and 15b, and are stopped in the concentrating chambers 15a and 15b by the anion exchange membranes 11a and 11 b; acid anions (sulfate, carbonate, chloride, etc.) pass through anion exchange membranes 11a, 11b into concentrating compartments 15a, 15b and are blocked by cation exchange membranes 12a, 12b and stay in concentrating compartments 15a, 15 b.
In one embodiment, the concentrated solution in the concentrating compartments 15a, 15b is discharged when the concentration of 1, 5-pentanediamine in the solution in the concentrating compartments 15a, 15b is not less than 5 wt%, and further not less than 7 wt%.
In one embodiment, the concentration of 1, 5-pentanediamine in the concentrated solution to be extracted introduced into the desalting chamber 16 is 0.1 to 5 wt%, and further 0.1 to 3 wt%;
in one embodiment, when the concentration of 1, 5-pentanediamine in the solution in the concentration chamber is 5 to 17 wt%, and further 8 to 15 wt%, the solution in the concentration chambers 15a and 15b is discharged to obtain a concentrated solution.
In one embodiment, the membrane pair voltage is 0.3-5V, and further 0.5-4V during the electrodialysis concentration treatment; controlling the current density to be 25-300A/m2Further, one is 25 to 150A/m2Further, one is 30 to 150A/m2Further, one is 150 to 250A/m2. The temperature is 10-60 ℃, further 10-40 ℃, and further 30-40 ℃; the linear velocity of each membrane surface of the electrodialysis device is 5-10 cm/s, and further 7-10 cm/s. In the electrodialysis concentration treatment process, polar liquid is introduced into the cathode chamber and the anode chamber, and the polar liquid comprises sulfuric acid solution and sulfate solution, such as sodium sulfate solution; the concentration of the polar liquid can be 2-5 wt%.
In one embodiment, the extraction unit includes a distillation apparatus, and further may be a vacuum distillation apparatus, to extract 1, 5-pentanediamine from an aqueous solution containing the 1, 5-pentanediamine by distillation.
The utility model discloses in, the vacuum distillation device can be the conventional distillation plant in this field, for example: a distillation column.
In one embodiment, the distillation temperature may be 100 to 180 ℃, and further may be 110 to 160 ℃.
In one embodiment, the pressure of the distillation may be 0MPa to 0.1MPa (absolute pressure).
In one embodiment, the extraction unit may further comprise a rectifying tower, and the rectifying tower may be disposed after the distillation device or downstream of the distillation device to further extract and refine the 1, 5-pentanediamine product obtained from the distillation device, so as to further improve the product quality.
The utility model discloses a 1, 5-pentanediamine extraction system of embodiment, during the operation, with first mixture through solid-liquid separation unit removal thallus, then through the adsorption unit in order to reduce metal ion content in the mixture, through the processing of bipolar membrane electrodialysis device, obtain the aqueous solution that contains 1, 5-pentanediamine;
in addition, concentrating the remaining second mixture in the salt chamber 7 after the treatment by the bipolar membrane electrodialysis device, recycling the concentrated solution to the salt chamber 7 of the bipolar membrane electrodialysis device, and further performing the bipolar membrane electrodialysis treatment to obtain an aqueous solution containing 1, 5-pentanediamine;
the aqueous solution containing 1, 5-pentanediamine obtained above is distilled in a vacuum distillation apparatus to obtain 1, 5-pentanediamine.
In one embodiment, the aqueous solution comprising 1, 5-pentanediamine comprises 1, 5-pentanediamine and water.
In one embodiment, when the system contains excessive pigment, protein, bacteria and metal ion impurities, the bottom of the distillation column in the distillation treatment of the extraction unit is sticky, and the mass and heat transfer efficiency is affected. Meanwhile, a part of 1, 5-pentamethylene diamine carried by the distillation residue can not be evaporated, and the product yield is influenced.
In one embodiment, the discharged low-concentration 1, 5-pentanediamine salt solution is treated by an electrodialysis concentration apparatus to further remove impurities such as pigments remaining in the 1, 5-pentanediamine salt solution. Compared with the prior art, the utility model discloses an embodiment's 1, 5-pentanediamine's extraction system, the material can form a closed loop during the operation, need not additionally to add alkali, has reduced sewage and the treatment cost who gives up admittedly.
The utility model relates to an embodiment's extraction system adopts bipolar membrane electrodialysis device separation purification 1, 5-pentanediamine, compares with current device, need not additionally to add alkali and other organic reagent, and the cost is reduced, and does not have solid useless and the high salt waste water that contains produces, has reduced the environmental protection pressure.
The utility model discloses an extraction system of embodiment can effectively get rid of impurity such as thallus, molecular protein, pigment, metal salt in the first mixture, and the obtained aqueous solution that contains 1, 5-pentanediamine purity is high, at more than 99.5% to 1, 5-pentanediamine's yield is high, and the yield is at more than 95%.
The utility model relates to an embodiment's extraction system, when producing 1, 5-pentanediamine, but recovery acid solution, can get back to fermentation link cyclic utilization once more after the acid solution of recovery is simply handled, and whole system almost has no waste residue waste discharge, and is very friendly to the environment.
The utility model relates to an embodiment's extraction system, easy operation, degree of automation is high, has improved staff's operational environment.
The following will further explain an extraction system of 1, 5-pentanediamine according to an embodiment of the present invention with reference to the drawings and specific examples. Wherein, the raw materials are all obtained from the market.
The test methods or calculation methods involved in the examples are as follows:
purity test of 1, 5-pentanediamine: measured by gas chromatography normalization method.
And (3) testing the content of metal ions: the test was performed using inductively coupled plasma atomic emission spectroscopy (ICP).
Example 1
Solid-liquid separation unit
Taking a first mixture, wherein the first mixture is fermentation liquor of 1, 5-pentanediamine, and contains sulfate of 1, 5-pentanediamine and carbonate of 1, 5-pentanediamine, the total concentration of the 1, 5-pentanediamine is 7.5 wt%, the thallus content is 1.7 wt%, the pH value is 8, and the color: brown; and (3) conveying the first mixture into a solid-liquid separation unit for centrifugal treatment, and filtering the centrifuged supernatant through a ceramic microfiltration membrane and an ultrafiltration membrane to obtain membrane clear liquid. Wherein the temperature of the ceramic microfiltration membrane in the filtration process is 31-34 ℃, the aperture of the ceramic microfiltration membrane is 0.05um, and the pressure difference between two sides of the membrane is 2 bar; the cutoff molecular weight of the ultrafiltration membrane is 3000Da, and the temperature of the ultrafiltration membrane in the filtering process is 31-34 ℃.
Adsorption unit
And (3) passing the membrane clear solution through a resin LXC500 (styrene-divinylbenzene framework, total exchange capacity of 6.6meq/ml) of an adsorption unit, the flow rate of the resin LXC500 is 4BV/h, the treatment capacity of the resin is 200BV, and collecting effluent liquid to obtain a second mixture.
Wherein, in the first mixture, the content of metal ions (calcium, magnesium and iron ions) is 56.76 ppm; in the second mixture, the metal ion content was 0.78 ppm. The metal ion removal rate was 98.63%, and the yield of 5-pentanediamine in the resin treatment step 1 was 99.90%.
The resin was regenerated using a 4 wt% hydrochloric acid solution.
Electrodialysis unit
And (3) introducing the second mixture obtained after the resin treatment into a salt chamber storage tank of the bipolar membrane electrodialysis device, and introducing a 3 wt% sulfuric acid solution into a polar chamber. Setting the upper limit of the membrane pair voltage of the bipolar membrane electrodialysis device to be 2.5V and controlling the current density to be 500A/m2Linear velocity of the film surface is 3cm/s, and controlling the temperature to be 30-40 ℃ in the bipolar membrane electrodialysis process.
Monitoring the bipolar membrane electrodialysis device, and discharging the residual 1, 5-pentanediamine salt solution in the salt chamber liquid storage tank to the electrodialysis concentration device when the conductivity of the solution in the salt chamber 7 is lower than 18mS/cm or the concentration of the 1, 5-pentanediamine is lower than 1.5 wt%.
When the conductivity of the solution in the alkali chamber 6 is higher than 4.2mS/cm or the concentration of the pentamethylene diamine is higher than 10 wt%, discharging and collecting the 1, 5-pentamethylene diamine aqueous solution in the alkali chamber liquid storage tank. And when the conductivity of the solution in the acid chamber 8 is higher than 400mS/cm or the acid radical concentration is higher than 1mol/L, discharging the acid solution in the acid chamber liquid storage tank.
And (3) subjecting the residual second mixture discharged from the salt chamber liquid storage tank to electrodialysis concentration treatment: and (3) introducing the second mixture to be concentrated into a weak room storage tank of the electrodialysis concentration device, and introducing a 3 wt% sulfuric acid solution into a polar room. Controlling the upper limit of the membrane pair voltage of the electrodialysis concentration device to be 0.5V and the current density to be 50A/m2The linear velocity of the membrane surface is 7cm/s, and the temperature during electrodialysis concentration is controlled to be 30-40 ℃.
When the concentration of 1, 5-pentanediamine in the solution in the concentrating compartments 15a, 15b reaches 9.62 wt%, the concentrated solution is discharged to obtain a concentrated second mixture. And recycling the concentrated second mixture to a bipolar membrane electrodialysis device, and carrying out bipolar membrane electrodialysis treatment to obtain an aqueous solution containing 1, 5-pentanediamine.
Extraction unit
And (3) introducing the aqueous solution containing the 1, 5-pentanediamine obtained by the bipolar membrane electrodialysis treatment into a distillation tower, and distilling at 110 ℃ and 500Pa absolute pressure to remove water to obtain the 1, 5-pentanediamine product, wherein the purity of the 1, 5-pentanediamine product is 99.5 wt%, and the content of metal ions is 0.65 ppm. The amount of residue after distillation was 4.81% by weight based on the mass of 1, 5-pentanediamine, and the yield was 95.4%.
The power consumption of the whole process is 1854kwh/t of products.
Example 2
Electrodialysis unit
The solution of 1, 5-pentanediamine salt (second mixture) treated by the solid-liquid separation unit and the adsorption unit in example 1 was introduced into the bipolarIn a salt chamber storage tank of the membrane electrodialysis device, 3 wt% sulfuric acid solution is introduced into an electrode chamber. Setting the upper limit of the membrane pair voltage of the bipolar membrane device to be 2.5V, and controlling the current density to be 500A/m2The linear velocity of the membrane surface is 3cm/s, and the temperature is controlled to be 30-40 ℃ in the bipolar membrane electrodialysis process.
The bipolar membrane electrodialysis unit was monitored and the aqueous solution of 1, 5-pentanediamine in the alkaline compartment solution reservoir was drained and collected when the conductivity of the solution in the salt compartment 7 no longer decreased. The solution remaining in the salt compartment 7 is drained into a sump.
Extraction unit
And (3) introducing the aqueous solution containing the 1, 5-pentanediamine obtained by the bipolar membrane electrodialysis treatment into a distillation tower, and distilling at 110 ℃ under the absolute pressure of 500Pa to remove water to obtain the 1, 5-pentanediamine product. The purity of the 1, 5-pentanediamine product was 99.3 wt%, and the metal ion content was 0.74 ppm. The amount of residue after distillation was 7.91% by weight based on the amount of 1, 5-pentanediamine, and the yield was 93.7%. The power consumption of the whole process is 4391kwh/t of product.
Unless otherwise defined, all terms used in the present invention have the meanings commonly understood by those skilled in the art.
The described embodiments are for illustrative purposes only and are not intended to limit the scope of the present invention, and various other substitutions, changes and modifications may be made by those skilled in the art within the scope of the present invention.
Claims (8)
1. An extraction system for 1, 5-pentanediamine for extracting 1, 5-pentanediamine from a first mixture, the extraction system comprising:
the adsorption unit is used for adsorbing the metal ions in the first mixture to obtain a second mixture;
an electrodialysis unit, which is used for carrying out electrodialysis treatment on the second mixture to obtain an aqueous solution containing 1, 5-pentanediamine; and
an extraction unit for separating 1, 5-pentanediamine from the aqueous solution containing 1, 5-pentanediamine;
wherein the adsorption unit is provided with resin, and the electrodialysis unit is provided with a bipolar membrane electrodialysis device.
2. The extraction system according to claim 1, comprising a solid-liquid separation unit disposed upstream of the adsorption unit for subjecting the first mixture to a solid-liquid separation treatment.
3. The extraction system according to claim 2, wherein a centrifugal device and/or a membrane filtration device is provided in the solid-liquid separation unit, and a microfiltration membrane and/or an ultrafiltration membrane is provided in the membrane filtration device.
4. The extraction system according to claim 1, wherein the bipolar membrane electrodialysis device comprises a first bipolar membrane, a second bipolar membrane, a cation exchange membrane and an anion exchange membrane, the cation exchange membrane and the anion exchange membrane being located between the first bipolar membrane and the second bipolar membrane, a base compartment being formed between the cation exchange membrane and the first bipolar membrane, an acid compartment being formed between the anion exchange membrane and the second bipolar membrane, and a salt compartment being formed between the cation exchange membrane and the anion exchange membrane.
5. The extraction system according to claim 4, wherein the electrodialysis unit further comprises a concentration device for concentrating the second mixture remaining in the salt compartment.
6. The extraction system according to claim 5, wherein the concentration device is selected from an evaporative concentration device and/or an electrodialysis concentration device.
7. The extraction system according to claim 1, wherein the extraction unit comprises a distillation apparatus.
8. The extraction system according to claim 7, wherein the extraction unit further comprises a rectification column for further purifying the 1, 5-pentanediamine product separated by the distillation apparatus.
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