CN1191220C - Process for desalting 1,3-propylene glycol fermentation liquor by electricity dialysis - Google Patents
Process for desalting 1,3-propylene glycol fermentation liquor by electricity dialysis Download PDFInfo
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- CN1191220C CN1191220C CNB031048714A CN03104871A CN1191220C CN 1191220 C CN1191220 C CN 1191220C CN B031048714 A CNB031048714 A CN B031048714A CN 03104871 A CN03104871 A CN 03104871A CN 1191220 C CN1191220 C CN 1191220C
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Abstract
The present invention discloses a process for desalting 1, 3-propanediol fermentation liquid by an electric dialysis process, which relates to the technical field of the desalinization of the 3-propanediol fermentation liquid, particularly to the technical field of the desalinization of the 3-propanediol fermentation liquid by the electric dialysis process. The process is characterized in that in the selection of main parameters, the initial concentration of a salt solution filled into a strong chamber tank is from 0.01 mol/L to 0.05 mol/L; the flow speed of the 3-propanediol fermentation liquid in a weak chamber is from 40 L/h to 80 L/h; the flow speed of the salt solution in a strong chamber is from 40 L/h to 80 L/h; the voltage of a single film pair is from 0.5V to 1.4V. The method can effectively eliminate an organic acid salt and an inorganic salt in 1, 3-propanediol, so the product loss rate is greatly reduced, and subsequent extraction operation is easy.
Description
Technical field:
Electroosmose process is used for 1, and the desalinating process of ammediol fermented liquid relates to the desalting technology field of fermented liquid, refers more particularly to the desalting technology field of electroosmose process to fermented liquid.
Background technology:
1, ammediol is a kind of important chemical material, mainly as the monomer of producing polyester and polyurethane.Fermentative Production 1, ammediol because of with low cost, reaction conditions is gentle, has become the focus that domestic and international investigator pays close attention in recent years.But can generate organic acid by products such as acetate, lactic acid during the fermentation, thereby make the reduction of fermented liquid pH value suppress the growth of thalline, cause 1, the ammediol productive rate is low excessively.Therefore, need in fermentation is carried out, add potassium hydroxide and regulate pH value normal growth with the assurance thalline about 7.The potassium hydroxide that adds can generate organic acid salt with organic acid, adds a certain amount of inorganic salt that itself comprises in the nutrient solution, make that fermentation obtains 1, have relatively large organic acid salt and inorganic salt in the ammediol product liquid.1, in the subsequent extracted of the vacuum distillation method of ammediol dehydration, the existence of salt can cause that the vacuum distilling temperature constantly raises, energy consumption increases; Along with salt is separated out meeting with part 1 with solid form, the ammediol product is wrapped in wherein, causes the product loss rate more than 20%; The enrichment factor of product is not higher than 30%-40% simultaneously.Therefore effectively remove 1, a large amount of organic acid salts and the inorganic salt that exist in the ammediol become 1, the part of key in the subsequent extracted of ammediol.Still the pertinent literature that does not have both at home and abroad at present effectively to address this problem is reported.
Electrodialytic technique is one of effective ways of separate electrolyte and nonelectrolyte, application at aspects such as sea water desaltination, fresh water purifying is very ripe, this method can not cause environmental pollution in application, and cost is comparatively cheap, also progressively is applied to separation, the recovery of organic acid and organic acid salt in the fermented liquid in recent years.Usually electroosmose process is used for fermented liquid, mainly is organic acid or the organic acid salt that removes as principal product, for example in the fermentative Production lactic acid process by electrodialytic technique with other separating substances (Li Xuemei etc. in lactic acid and the fermented liquid.The electroosmose process of Lactic Acid from Fermentation Broth separates.Colleges and universities' chemical engineering journal, 1998,12 (3): 231-235), by electrodialytic technique Sodium.alpha.-hydroxypropionate is converted into lactic acid (L.Madzingaidzo etc. in the fermentative Production lactic acid process.Process development and optimisation of lactic acid purification usingelectrodialysis.Journal of biotechnology, 2002,96:223-239) etc.Be used for the technological operation of fermented liquid at electroosmose process, at different operands, its processing condition and operating parameters all have very big-difference, 1, in the desalinating process of ammediol fermented liquid, salt is removed from fermented liquid as by product, both at home and abroad not research as yet at present with electroosmose process.
Summary of the invention:
The present invention is directed to 1, the characteristics of ammediol have proposed electroosmose process and have been used for 1, the desalinating process of ammediol fermented liquid, and this method can effectively remove 1, and organic acid salt in the ammediol fermented liquid and inorganic salt can reduce the product losses rate greatly.
The present invention contains following steps:
1) in light chamber jar (7), pack into pending 1, ammediol fermented liquid, the salts solution of in dense chamber jar (4), packing into, the acid solution of in anolyte compartment's jar (6), packing into, the alkaline solution of in cathode compartment jar (5), packing into;
2) open the pump (8A) of controlling above-mentioned dense chamber jar (4), control the pump (8D) of above-mentioned light chamber jar (7), control the pump (8C) of above-mentioned anolyte compartment jar (6), control the pump (8B) of above-mentioned cathode compartment jar (5), make above-mentioned salts solution, 1, ammediol fermented liquid, acid solution, alkaline solution circulate in electrodialyzer; By regulating the flow velocity of the above-mentioned salts solution of under meter (9A) control, above-mentioned 1 by regulating under meter (9D) control, the flow velocity of ammediol fermented liquid; By regulating the flow velocity of the above-mentioned alkaline solution of under meter (9B) control; By regulating the flow velocity of the above-mentioned acid solution of under meter (9C) control;
3) open and regulate direct supply (2), for monofilm to adding voltage, make electrodialyzer work;
4) close direct supply (2) and pump (8A-8D);
It is characterized in that the above-mentioned the 1st) in the step, the starting point concentration of the salts solution of packing in the described dense chamber jar (7) is 0.01mol/L～0.05mol/L; The above-mentioned the 2nd) in the step, described 1, the flow rate regulation of ammediol fermented liquid is 40L/h～80L/h, and the flow rate regulation of described salts solution is 40L/h～80L/h; The above-mentioned the 3rd) in the step, regulating direct supply (2) is 0.5V～1.4V for monofilm to the voltage that adds.
Experiment showed, and use electroosmose process proposed by the invention to be used for 1, the desalinating process of ammediol fermented liquid, can effectively deviate from 1, organic acid salt in the ammediol and inorganic salt make in the subsequent extracted 1, the product loss rate of ammediol reduces greatly, has reached its intended purposes.
Description of drawings:
Fig. 1 is the work synoptic diagram of electrodialyzer used in the present invention.
Embodiment:
In conjunction with Fig. 1 the specific embodiment of the present invention is described.
Process unit used in the present invention mainly comprises electrodialyzer 1, D.C. regulated power supply 2, current meter 3, pump 8A-8D, under meter 9A-9D, as shown in Figure 1.Wherein, electrodialyzer 1 is conventional electrodialyzer, by 10 pairs of yin, yang ion-exchange membrane (monofilm areas: 100 * 300mm
2-400 * 1600mm
2) alternately form, wherein A is an anion-exchange membrane, and C is a cationic exchange membrane, and what the present invention adopted is anti-strong acid, the alkaline homogeneous ion-exchange membrane that the global profit in Beijing reaches environmental protection equipment company.
In the operating process, the starting point concentration of salts solution in the jar 4 of dense chamber, in the light chamber jar 71, the flow velocity of ammediol fermented liquid, the flow velocity of salts solution in the jar 4 of dense chamber, with the monofilm that applies be very crucial operating parameters to voltage, need by the desalination time in the actual demineralising process, energy consumption, the calculating of three indexs of ratio of desalinization relatively obtains optimum value, the present invention is by calculating 1, ammediol is in the electrodialytic desalting process, required energy consumption and desalination time are weighed desalting effect when reaching identical ratio of desalinization, determine the optimum range of above-mentioned Several Parameters simultaneously, the determining of ratio of desalinization size characterizes by measure the initial and final conductivity value of fermented liquid with conductivitimeter, and definite employing formula of energy consumption: energy consumption=operating voltage * electric current * operating time is determined.
Describe by following 8 groups of experiments:
Test 1:
1) in light chamber jar 7, packs pending 1 into, 3 liters of ammediol fermented liquids (recording its conductivity value is 15000 μ s/cm), the concentration of packing in the dense chamber jar 4 is 3 liters of the liquor kalii aceticis of 0.01mol/L, the concentration of packing in anolyte compartment's jar 6 is 2 liters of the sulphuric acid solns of 0.05mol/L, and the concentration of packing in the cathode compartment jar 5 is 2 liters of the sodium hydroxide solutions of 0.05mol/L.
2) open pump 8A-8D, make salts solution, 1, ammediol fermented liquid, acid solution, alkaline solution circulate in electrodialyzer 1, regulate under meter 9A and 9D, make in the dense chamber jar 4 in the liquor kalii acetici flow velocity and light chamber jar 71, ammediol fermented liquid flow velocity reaches 60L/h, regulates under meter 9B and 9C, make in the cathode compartment jar 5 that the sulphuric acid soln flow velocity reaches 40L/h in the sodium hydroxide solution flow velocity and anolyte compartment's jar 6, circulated 30 minutes.
3) open direct supply 2, be adjusted to 5V, making monofilm is 0.5V to last voltage, and electrodialyzer 1 is started working.
4) when conductivity value is reduced to 600 μ s/cm, close direct supply 2, close pump 8A-8D.The time that record electrodialysis work this moment is 16 hours.
Behind the EO, by calculating, obtaining the required energy consumption of electrodialytic desalting process is 5.36wh/L.
Below 7 groups the experiment in, the present invention has only changed in the starting point concentration of liquor kalii acetici in the jar 4 of dense chamber, the light chamber jar 71, the flow velocity of liquor kalii acetici and the right magnitude of voltage of monofilm in the flow velocity of ammediol fermented liquid, the dense chamber jar 4, all the other parameters are all constant, when reaching same electrical conductance (specific conductivity is reduced to 600s/cm from 15000s/cm), measure its used time, and calculate energy consumption.8 groups of data of experiment gained are as shown in table 1.
| Group | Salts solution starting point concentration (mol/L) in the jar of dense chamber | Fermented liquid flow velocity (L/h) in the light chamber | Salts solution flow velocity (L/h) in the jar of dense chamber | Monofilm is to voltage (V) | Working hour (h) | Energy consumption (wh/L) |
| 1 | 0.01 | 60 | 60 | 0.5 | 16 | 5.36 |
| 2 | 0.01 | 60 | 60 | 0.7 | 12 | 7.01 |
| 3 | 0.01 | 60 | 60 | 1.0 | 9 | 11.12 |
| 4 | 0.01 | 60 | 60 | 1.4 | 6 | 16.9 |
| 5 | 0.03 | 60 | 60 | 0.7 | 11.5 | 8.67 |
| 6 | 0.05 | 60 | 60 | 0.7 | 13 | 8.68 |
| 7 | 0.05 | 40 | 40 | 0.7 | 12 | 7.52 |
| 8 | 0.05 | 80 | 80 | 0.7 | 12 | 7.68 |
Table 1
From table, can find out, the starting point concentration of salts solution is at 0.01～0.05mol/L in the jar 4 of dense chamber, in the jar of light chamber 1, the flow velocity of salts solution is at 40～80L/h in ammediol fermented liquid and the dense chamber jar, monofilm to added voltage when the 0.5V～1.4V, can make fermented liquid reach higher ratio of desalinization (specific conductivity), and when reaching identical ratio of desalinization, needed working hour and required energy consumption are all little.When monofilm was higher to voltage, required time was shorter, and energy consumption is big slightly; When the right voltage of monofilm was low, required time was longer, and energy consumption is less, but the required time reaches relative equilibrium with consuming energy.
In the electrodialytic desalting process, the starting point concentration of positive and negative utmost point chamber, wherein the flow velocity of bronsted lowry acids and bases bronsted lowry solution is little to the influential effect of desalination, and can select the parameter area of using always in the electrodialysis process of fermented liquid: anolyte compartment and cathode compartment flow velocity are 20L/h-60L/h; The concentration of acid solution and alkali lye is 0.01mol/L-0.1mol/L in anolyte compartment and the cathode compartment.
With in the high-performance liquid chromatogram determination fermented liquid 1, after the starting point concentration C1 of ammediol and the desalination 1, the ammediol concentration C
2, calculate 1, ammediol rate of loss ((C
1-C
2)/C
1) only be 4.5%-6.0%.After this technology desalting treatment 1, when art breading such as distillation, enrichment factor can disposablely reach more than 70% the ammediol fermented liquid again.
Proof adopts the suitable parameters scope by experiment, removes 1 with electroosmose process, and the by-product salt in the ammediol fermented liquid can reach obvious effects, makes subsequent extracted work more smooth.
Claims (1)
1, electroosmose process is used for 1, and the desalinating process of ammediol fermented liquid contains following steps:
1) in light chamber jar (7), pack into pending 1, ammediol fermented liquid, the salts solution of in dense chamber jar (4), packing into, the acid solution of in anolyte compartment's jar (6), packing into, the alkaline solution of in cathode compartment jar (5), packing into;
2) open the pump (8A) of controlling above-mentioned dense chamber jar (4), control the pump (8D) of above-mentioned light chamber jar (7), control the pump (8C) of above-mentioned anolyte compartment jar (6), control the pump (8B) of above-mentioned cathode compartment jar (5), make above-mentioned salts solution, 1, ammediol fermented liquid, acid solution, alkaline solution circulate in electrodialyzer; By regulating the flow velocity of the above-mentioned salts solution of under meter (9A) control, above-mentioned 1 by regulating under meter (9D) control, the flow velocity of ammediol fermented liquid; By regulating the flow velocity of the above-mentioned alkaline solution of under meter (9B) control; By regulating the flow velocity of the above-mentioned acid solution of under meter (9C) control;
3) open and regulate direct supply (2), for monofilm to adding voltage, make electrodialyzer work;
4) close direct supply (2) and pump (8A-8D);
It is characterized in that the above-mentioned the 1st) in the step, the starting point concentration of the salts solution of packing in the described dense chamber jar (7) is 0.01mol/L～0.05mol/L; The above-mentioned the 2nd) in the step, described 1, the flow rate regulation of ammediol fermented liquid is 40L/h～80L/h, and the flow rate regulation of described salts solution is 40L/h～80L/h; The above-mentioned the 3rd) in the step, regulating direct supply (2) is 0.5V～1.4V for monofilm to the voltage that adds.
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|---|---|---|---|
| CNB031048714A CN1191220C (en) | 2003-02-21 | 2003-02-21 | Process for desalting 1,3-propylene glycol fermentation liquor by electricity dialysis |
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| CNB031048714A CN1191220C (en) | 2003-02-21 | 2003-02-21 | Process for desalting 1,3-propylene glycol fermentation liquor by electricity dialysis |
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| CN101108194B (en) * | 2007-06-30 | 2010-12-01 | 广西壮族自治区化工研究院 | Method of eliminating sodium chloride in iron-dextran complex compound water solution and device thereof |
| CN101117306B (en) * | 2007-07-20 | 2011-01-19 | 三达膜科技（厦门）有限公司 | Methods for edulcoration and desalinization of 1,3-methyl glycol fermentation liquor |
| CN101298409B (en) * | 2008-01-23 | 2010-11-10 | 湖南海纳百川生物工程有限公司 | Electrodialysis desalination process using heterophase ion-exchange membrane to 1, 3-propanediol fermentation liquor |
| MX2011003558A (en) | 2008-10-03 | 2011-05-02 | Metabolic Explorer Sa | Method for purifying an alcohol from a fermentation broth using a falling film, a wiped film, a thin film or a short path evaporator. |
| CN105838771B (en) * | 2015-01-16 | 2019-09-27 | 上海凯鑫分离技术股份有限公司 | Amoxicillin crystalline mother solution recovery process |
| CN106349055B (en) * | 2016-08-24 | 2017-12-01 | 山东福洋生物科技有限公司 | A kind of new separating and extracting process of gluconic acid mother liquid of sodium |
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