CN101691349A - Process for extracting tryptophan from fermentation liquid - Google Patents
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- CN101691349A CN101691349A CN200910019458A CN200910019458A CN101691349A CN 101691349 A CN101691349 A CN 101691349A CN 200910019458 A CN200910019458 A CN 200910019458A CN 200910019458 A CN200910019458 A CN 200910019458A CN 101691349 A CN101691349 A CN 101691349A
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Abstract
The invention provides a new clean production process of tryptophan. In the method, the fermentation liquid of the tryptophan is taken as the raw material, and the high purity tryptophan is obtained by the steps of acidifying, ceramic membrane filter washing, organic membrane ultrafiltration, intermittent concentration and crystallization, centrifugal separation and drying, the ion exchange desalination technology is adopted to process crystallization mother liquid and the products are recycled, thus improving the product yield. The process not only overcomes the defects of traditional long process routes and complicated step of needing a large number of organic solvents for recrystallization, but also is more favorable to process production and reduces the environmental pollution in production.
Description
Technical field
The present invention relates to a kind of production method of tryptophane, be specially a kind of technology of from fermented liquid, extracting tryptophane.
Background technology
Tryptophane, English name: Tryptophan, chemical name: L-2-amino-3 (β-indoles) propionic acid, chemical formula: C
11H
12N
2O
2, formal name used at school: tryptophane (β-indolylalanine).It has three kinds of isomer.Its raceme is a white crystal, is slightly soluble in water, and is stable in basic solution, decomposed by strong acid; Levo form is white or little yellow tabular crystal, odorless, mildly bitter flavor.289 ℃ of fusing points (decomposition), slightly soluble in water, soluble,very slightly in ethanol, insoluble in chloroform, easily molten in formic acid, in sodium hydroxide test solution or dilute hydrochloric acid, dissolve; Dextrorotatory form is a white crystal, and special sweet taste is arranged, fusing point 281-282 ℃ (decomposition), water-soluble, hot ethanol and alkali hydroxide solution.
The L-tryptophane is a heterocyclic amino acid, be one of human body and necessary 8 seed amino acids of animal life activity, be important nutrition agent, be widely used in amino acid transfusion, comprehensive amino acid preparation, nutritious supplementary, pellagra treatment, tranquilizer (regulate the spiritual rhythm and pace of moving things, improve sleep), food and feed additive.In recent years, along with the continuous development of domestic and international fodder industry and medicine industry, tryptophane becomes the product that a kind of world market development prospect is good, the Chinese market demand is bigger.The production of tryptophane mainly relies on chemical synthesis and proteolysis method the earliest, but along with microbial method being produced deepening continuously of tryptophane research, this method has been moved towards practical and has been in dominant position.Microbial method can be divided into direct fermentation, microbe transformation method and enzyme process substantially.Produce tryptophane suitability for industrialized production ability of certain scale with microorganism direct fermentation.Contain impurity such as a large amount of mycelium, albumen, pigment in the tryptophane fermented liquid that direct fermentation obtains, must could obtain purity height, tryptophane that transmittance is good by certain extraction and separation technology.
The extraction purification technique of tryptophane mainly adopts absorption and ion exchange method at present, passes through neutralization or cooling recrystallization in the presence of lower aliphatic alcohols, complex process.Adopt organic solvent to carry out the extraction of tryptophane simultaneously, increase solvent recuperation and post-processing difficulty, environment is caused disadvantageous effect.
Japanese Patent prospectus (JP895/1983) adopts tryptophane solution earlier by nonpolar porous resin, extract tryptophane by the method for ultrafiltration again, but Impurity removal is undesirable, does not reach the high transmission rate requirement.Japanese Patent prospectus (JP39857/1984) has proposed tryptophane and has dissolved with alkali lye, in the presence of low fat alcohol or ketone in and crystallization, improve purity, but Impurity removal is still insufficient, and transmittance is difficult to reach 95%, and, use a large amount of solvents, caused follow-up solvent treatment difficulty.Japanese Patent prospectus (JP126070/1986) is dissolved in tryptophane in 95-100 ℃ the acidic solution, after the carbon removal of charcoal absorption rate, again through nonpolar porous resin absorption, wash-out tryptophane, in in the presence of low lipidol and crystal, transmittance is also undesirable.In the US Patent specification (US5057615), tryptophane in 40-115 ℃ aqueous acetic acid, is used activated carbon adsorption earlier, decrease temperature crystalline behind the de-carbon exists tryptophane to decompose discoloration problem equally.Domestic tryptophane purification technique report is less, mostly adopts ion exchange resin absorption tryptophane, and the defective of this method is: tryptophane is easy to oxidation, the yield instability; Extraction tryptophane impurity is more, color and luster is dark; Water loss is big, and the soda acid consumption is big, can produce a large amount of waste residues and waste water, contaminate environment aborning.
In sum, in the extraction process of tryptophane, mostly exist at present both at home and abroad tryptophane degraded, decolouring not thoroughly, to the pollution of environment, the handling problem of follow-up organic solvent etc.
Summary of the invention
In order to overcome the shortcoming that exists in the existing tryptophane extraction process, the invention provides a kind of tryptophane new cleanproduction process, the present invention is a raw material with the tryptophane fermented liquid, obtain highly purified tryptophane through acidifying, ceramic membrane filter wash, organic membrane ultrafiltration, batch concentration crystallization, centrifugation and drying process step, and adopt the circulation of ion-exchange demineralization technical finesse crystalline mother solution to reclaim product, improve product yield.It is not only beaten traditional operational path length, must carry out the loaded down with trivial details step of recrystallization with a large amount of organic solvents, and makes this technology help technology production more, reduces the pollution of environment in producing.
Technical scheme of the present invention is: a kind of technology of from fermented liquid, extracting tryptophane, and its processing step is:
(1) online heating dilution acidifying technology is carried out the adjusting of fermented liquid pH value
With 1 times of fermented liquid thin up, and fermented liquid is heated to temperature is 50-100 ℃, adopt static mixed technology, adding concentration is the sulfuric acid of 70-98%, regulate pH to 3-6 by control fermented liquid and vitriolic flow proportional, tryptophane is present in the fermented liquid with solution state, and makes the tropina sex change, be suitable for thalline and separate;
(2) the continuous online filter wash of ceramic membrane
To through the ceramic membrane on-line filtration, remove the whole mycelium in the fermented liquid through step (1) acidifying fermented liquid; Described ceramic membrane membrane pore size is 50nm, and the filtering service temperature of controlling diaphragm is 50-90 ℃, and advancing film pressure is 1.5-3.0bar, filters out the bacterium slag, and the stock liquid volume is concentrated into 8-15 times of bacterium slag volume, and spray is dried can do tropina to the bacterium slag through concentrating;
(3) the rolling organic membrane removes albumen, macromole impurity, decolouring
To remove Deproteinization, macromole impurity and pigment through the rolling organic membrane through the feed liquid behind step (2) filter wash, the described rolling organic membrane molecular weight that can dam is 1000, control pH 2.0-5.0, filtration temperature is 20-40 ℃, controlled filter pressure 10-20bar, the feed liquid transmittance obviously improves after the organic membrane decolouring, is risen to more than 95% by original 9-10%;
(4) batch concentration crystallization
Adopt the triple effect falling liquid film to concentrate, 60-90 ℃ of thickening temperature imitated in control one, 90-110 ℃ of thickening temperature imitated in control two, 50-80 ℃ of control triple effect thickening temperature, the control vacuum pressure be-0.08Mpa is above (the most very much not can be surpassed-0.1Mpa), will be concentrated to state of saturation through the feed liquid after step (3) organic membrane decolours; Then concentrated solution is delivered to the Concentrated and crystallized in vacuum jar immediately, 50-75 ℃ of vacuum concentration temperature, more than vacuum pressure-0.08Mpa (the most very much not can surpass-0.1Mpa), continuing to be concentrated into feed liquid proportion is 1.15-1.4g/cm
3Add ammoniacal liquor then and regulate pH to 4.5-6.8, nature decrease temperature crystalline under the normal pressure, crystallization control process time are 2-6 hour; After crystal was separated out, the new concentrated solution of restock was warmed up to 50-75 ℃ to original volume (volume that adds the concentrated solution of condensing crystal jar for the first time), and vacuum concentration to feed liquid proportion is 1.15-1.4g/cm
3, ammoniacal liquor is regulated pH to 4.5-6.8, nature decrease temperature crystalline under the normal pressure, and three additional concentrated solutions like this, being concentrated into volume at last is the 30-40% of original volume (volume that adds the concentrated solution of condensing crystal jar for the first time), obtains sheet tryptophane crystal;
(5) adopt dull and stereotyped centrifuge with cutter discharge of solid to dry and separate the removal crystalline mother solution, collect the tryptophane crystal, it is the product tryptophane that drying obtains white crystalline powder;
(6) crystalline mother solution utilizes macropore cation resin to carry out the desalination processing, crystalline mother solution mixes in 1: 0.5 ratio with pure water, control pH5.5-6.5,35 ℃ of working temperatures, ion exchange column bed length-to-diameter ratio is 6: 1, and the charging flow velocity per hour is that flow is 1.5 times of column volume, and effluent liquid returns ceramic membrane membrane filtration process circular treatment again, reclaim product, the inorganic salt of wash-out and heteroacid can be done the mineral manure sale also can do the fermention medium batching.
Tryptophane is 30-50g/L in the used tryptophane fermented liquid of the present invention, and the pH value is 4.0-7.0, and residual sugar is below the 0.5g/L, and it is to be that raw material adopts the fermented liquid that direct fermentation was obtained with glucose etc., and the tryptophane zymotechnique belongs to prior art.
Gained tryptophane of the present invention is a white crystalline powder, odorless, and mildly bitter flavor, its performance index are as shown in table 1.
Table 1 adopts the performance index of the tryptophane of this explained hereafter
| Project | Index |
| Tryptophane (in butt), % 〉= | ??98.5 |
| Specific rotation [a] 20D | ??-29.5°～-33.0° |
| Weight loss on drying, %≤ | ??0.5 |
| Calcination is residual, %≤ | ??0.5 |
| Heavy metal (in Pb), %＜ | ??0.002 |
| Arsenic (in As), %＜ | ??0.0002 |
The invention has the beneficial effects as follows: technology advanced person of the present invention, quality product height.Be specially: 1) online heating dilution acidifying technology, adopt static mixer, regulate the pH value continuously, reduce investment outlay and stir power charge; 2) adopt the online filter wash technology of ceramic membrane, improve the quality of products and yield, chemistry that ceramic membrane is good and mechanical property, are easy to clean and maintenance at high temperature resistant, acid and alkali-resistance; Compare other separating device, improved cycles of concentration, reduce the discharging of bacterium slag.The bacterium slag that filters out can be done tropina through concentrating; 3) adopt the rolling organic membrane to remove albumen, macromole impurity and decolouring, improve the filtrate quality, make filtrate purer, bright, foreign matter content is lower, improves the quality of products; 4) the batch concentration crystallization processes need not granulation, and direct crystallization obtains the plate crystal body, improves product purity, color and luster brightness, no static.Primary crystallization can satisfy the demand of feed grade, food grade products.5) crystalline mother solution returns the membrane filtration cycle of treatment again through ion-exchange demineralization, reclaims product, improves product yield, reduces production costs.The inorganic salt that reclaim can be sold and make fertilizer and maybe can do the fermentation culture batching; 6) process for cleanly preparing of whole tryptophane zymotechnics is the closed loop extraction process, and three waste discharge is few.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Below further specify technical scheme of the present invention by specific embodiment.
Embodiment 1
(1) (tryptophane is 40g/L with the 500L fermented liquid, pH value is 6.0, residual sugar is 0.5g/L) thin up is to 1000L, and fermented liquid is heated to temperature is 70 ℃, adopts static mixed technology, and adding concentration is the sulfuric acid of 70-98%, regulate pH to 4.0 by control fermented liquid and vitriolic flow proportional, tryptophane is present in the fermented liquid with solution state, and makes the tropina sex change, be suitable for thalline and separate;
(2) will through the online filter wash of ceramic membrane, remove the whole mycelium in the fermented liquid through step (1) acidifying fermented liquid; Described ceramic membrane membrane pore size is 50nm, and the filtering service temperature of controlling diaphragm is 70 ℃, and advancing film pressure is 2.0bar, and the stock liquid volume is concentrated into 10 times of bacterium slag volume, and spray is dried can do tropina to the bacterium slag through concentrating;
(3) will remove Deproteinization, macromole impurity and pigment through the rolling organic membrane through the feed liquid behind step (2) filter wash, the organic membrane molecular weight that dams is 1000, control pH 4.0, and filtration temperature is 30 ℃, controlled filter pressure 15bar;
(4) adopt the triple effect falling liquid film concentrated, control one and imitate 70 ℃ of thickening temperatures, 100 ℃ of thickening temperatures are imitated in control two, control 70 ℃ of triple effect thickening temperatures, control vacuum pressure to be-more than the 0.08Mpa, will be concentrated to state of saturation through the feed liquid after the decolouring of step (3) organic membrane; Then concentrated solution is delivered to the Concentrated and crystallized in vacuum jar immediately, 70 ℃ of vacuum concentration temperature, vacuum pressure is-more than the 0.08Mpa, being concentrated into feed liquid proportion is 1.2g/cm
3, adding ammoniacal liquor then and regulate pH 6.0, nature decrease temperature crystalline under the normal temperature, crystallization control process time are 3 hours; After crystal was separated out, the new concentrated solution of restock was warmed up to 70 ℃ to original volume, and vacuum concentration to feed liquid proportion is 1.2g/cm
3, ammoniacal liquor is regulated pH to 6.0, nature decrease temperature crystalline under the normal pressure, and three additional concentrated solutions like this, concentrating volume at last is the 30-40% of original volume, obtains sheet tryptophane crystal;
(5) adopt dull and stereotyped centrifuge with cutter discharge of solid to dry and separate the removal crystalline mother solution, collect the tryptophane crystal, it is the product tryptophane that drying obtains white crystalline powder;
(6) crystalline mother solution utilizes the ion-exchange demineralization technical finesse, crystalline mother solution mixes in 1: 0.5 ratio with pure water, control pH5.5-6.5,35 ℃ of working temperatures, ion exchange column bed length-to-diameter ratio is 6: 1, and the charging flow velocity per hour is that flow is 1.5 times of column volume, returns ceramic membrane membrane filtration process circular treatment again, reclaim product, the inorganic salt of recovery can be done the mineral manure sale also can do the fermention medium batching.
Product tryptophane yield is 99.8%, and the every index of product tryptophane all meets the tryptophane performance index shown in the table 1.
Embodiment 2
(1) (tryptophane is 35g/L with the 500L fermented liquid, the pH value is 5.5, residual sugar is 0.4g/L) thin up is to 1000L, and fermented liquid is heated to temperature is 50 ℃, adopts static mixed technology, and adding concentration is the sulfuric acid of 70-98%, regulate pH to 3 by control fermented liquid and vitriolic flow proportional, tryptophane is present in the fermented liquid with solution state, and makes the tropina sex change, be suitable for thalline and separate;
(2) will through the online filter wash of ceramic membrane, remove the whole mycelium in the fermented liquid through step (1) acidifying fermented liquid; Described ceramic membrane membrane pore size is 50nm, and the filtering service temperature of controlling diaphragm is 50 ℃, and advancing film pressure is 3.0bar.Concentrate stock liquid volume 15 times to bacterium slag volume, spray is dried can do tropina to the bacterium slag through concentrating;
(3) will remove Deproteinization, macromole impurity and pigment through the rolling organic membrane through the feed liquid behind step (2) filter wash, the film molecular weight that can dam is 1000, control pH 3, and filtration temperature is 20 ℃, controlled filter pressure 20bar;
(4) adopt the triple effect falling liquid film concentrated, control one and imitate 60 ℃ of thickening temperatures, 90 ℃ of thickening temperatures are imitated in control two, control 50 ℃ of triple effect thickening temperatures, control vacuum pressure to be-more than the 0.08Mpa, will be concentrated to state of saturation through the feed liquid after the decolouring of step (3) organic membrane; Then concentrated solution is delivered to the Concentrated and crystallized in vacuum jar immediately, 50 ℃ of vacuum concentration temperature, vacuum pressure is-more than the 0.08Mpa, being concentrated into feed liquid proportion is 1.4g/cm
3, adding ammoniacal liquor then and regulate pH 4.5, nature decrease temperature crystalline under the normal temperature, crystallization control process time are 4 hours; After crystal was separated out, the new concentrated solution of restock was warmed up to 50 ℃ to original volume, and vacuum concentration to feed liquid proportion is 1.4g/cm
3, ammoniacal liquor is regulated pH to 4.5, falls crystallization under the normal pressure naturally, three additional concentrated solutions like this, and concentrating volume at last is the 30-40% of original volume, obtains sheet tryptophane crystal;
(5) adopt dull and stereotyped centrifuge with cutter discharge of solid to dry and separate the removal crystalline mother solution, collect the tryptophane crystal, it is the product tryptophane that drying obtains white crystalline powder.
(6) crystalline mother solution utilizes the ion-exchange demineralization technical finesse, crystalline mother solution mixes in 1: 0.5 ratio with pure water, control pH5.5-6.5,35 ℃ of working temperatures, ion exchange column bed length-to-diameter ratio is 6: 1, and the charging flow velocity per hour is that flow is 1.5 times of column volume, returns ceramic membrane membrane filtration process circular treatment again, reclaim product, the inorganic salt of recovery can be done the mineral manure sale also can do the fermention medium batching.
The yield of product tryptophane is 99.5%, and the every index of product tryptophane all meets the tryptophane performance index shown in the table 1.
Embodiment 3
(1) (tryptophane is 40g/L with the 500L fermented liquid, pH value is 6.5, residual sugar is 0.4g/L) thin up is to 1000L, and fermented liquid is heated to temperature is 90 ℃, adopts static mixed technology, and adding concentration is the sulfuric acid of 70-98%, regulate pH value to 5 by control fermented liquid and vitriolic flow proportional, tryptophane is present in the fermented liquid with solution state, and makes the tropina sex change, be suitable for thalline and separate;
(2) will through the online filter wash of ceramic membrane, remove the whole mycelium in the fermented liquid through step (1) acidifying fermented liquid; Described ceramic membrane membrane pore size is 50nm, and the filtering service temperature of controlling diaphragm is 90 ℃, and advancing film pressure is 1.5bar, concentrates stock liquid volume 8 times to bacterium slag volume, the bacterium slag that filters out, and spray is dried can do tropina through concentrating;
(3) will remove Deproteinization, macromole impurity and pigment through the rolling organic membrane through the feed liquid behind step (2) filter wash, the film molecular weight that can dam is 1000, control pH 5.0, and filtration temperature is 40 ℃, controlled filter pressure 10bar;
(4) adopt the triple effect falling liquid film concentrated, control one and imitate 90 ℃ of thickening temperatures, 110 ℃ of thickening temperatures are imitated in control two, control 75 ℃ of triple effect thickening temperatures, control vacuum pressure to be-more than the 0.08Mpa, will be concentrated to state of saturation through the feed liquid after the decolouring of step (3) organic membrane; Then concentrated solution is delivered to the Concentrated and crystallized in vacuum jar immediately, 75 ℃ of vacuum concentration temperature, vacuum pressure is-more than the 0.08Mpa.Being concentrated into feed liquid proportion is 1.15g/cm
3, add ammoniacal liquor then and regulate pH 6.8, nature decrease temperature crystalline under the normal temperature, the crystallization control process time is 4 hours, and after crystal was separated out, the concentrated solution that restock is new was warmed up to 75 ℃, and vacuum concentration to feed liquid proportion is 1.15g/cm
3, ammoniacal liquor is regulated pH to 6.8, and nature decrease temperature crystalline under the normal pressure, three additional concentrated solutions like this are to original volume, and concentrating volume at last is the 30-40% of original volume, obtains sheet tryptophane crystal;
(5) adopt dull and stereotyped centrifuge with cutter discharge of solid to dry and separate the removal crystalline mother solution, collect the tryptophane crystal, it is the product tryptophane that drying obtains white crystalline powder.
(6) crystalline mother solution utilizes the ion-exchange demineralization technical finesse, crystalline mother solution mixes in 1: 0.5 ratio with pure water, control pH5.5-6.5,35 ℃ of working temperatures, ion exchange column bed length-to-diameter ratio is 6: 1, and the charging flow velocity per hour is that flow is 1.5 times of column volume, returns ceramic membrane membrane filtration process circular treatment again, reclaim product, the inorganic salt of recovery can be done the mineral manure sale also can do the fermention medium batching.
Product tryptophane yield is 99.3%, and the every index of product tryptophane all meets the tryptophane performance index shown in the table 1.
Embodiment 4
(1) (tryptophane is 40g/L with the 500L fermented liquid, the pH value is 6.0, residual sugar is 0.4g/L) thin up is to 1000L, and fermented liquid is heated to temperature is 60 ℃, adopts static mixed technology, and adding concentration is the sulfuric acid of 70-98%, regulate pH to 4.5 by control fermented liquid and vitriolic flow proportional, tryptophane is present in the fermented liquid with solution state, and makes the tropina sex change, be suitable for thalline and separate;
(2) will through the online filter wash of ceramic membrane, remove the whole mycelium in the fermented liquid through step (1) acidifying fermented liquid; Described ceramic membrane membrane pore size is 50nm, and the filtering service temperature of controlling diaphragm is 60 ℃, and advancing film pressure is 2.5bar, concentrates stock liquid volume 12 times to bacterium slag volume, and spray is dried can do tropina to the bacterium slag through concentrating;
(3) will remove Deproteinization, macromole impurity and pigment through the rolling organic membrane through the feed liquid behind step (2) filter wash, the film molecular weight that can dam is 1000, control pH 4.5, and filtration temperature is 25 ℃, controlled filter pressure 16bar;
(4) adopt the triple effect falling liquid film concentrated, control one and imitate 70 ℃ of thickening temperatures, 100 ℃ of thickening temperatures are imitated in control two, control 60 ℃ of triple effect thickening temperatures, control vacuum pressure to be-more than the 0.08Mpa, will be concentrated to state of saturation through the feed liquid after the decolouring of step (3) organic membrane; Then concentrated solution is delivered to the Concentrated and crystallized in vacuum jar immediately, 60 ℃ of vacuum concentration temperature, vacuum pressure is-more than the 0.08Mpa.Being concentrated into feed liquid proportion is 1.3g/cm
3Add ammoniacal liquor then and regulate pH 5.5, nature decrease temperature crystalline under the normal temperature, the crystallization control process time is 4 hours, and after crystal was separated out, the new concentrated solution of restock was warmed up to 60 ℃ to original volume, and vacuum concentration to feed liquid proportion is 1.3g/cm
3, ammoniacal liquor is regulated pH to 5.5, nature decrease temperature crystalline under the normal pressure, and three additional concentrated solutions like this, concentrating volume at last is the 30-40% of original volume, obtains sheet tryptophane crystal;
(5) adopt dull and stereotyped centrifuge with cutter discharge of solid to dry and separate the removal crystalline mother solution, collect the tryptophane crystal, it is the product tryptophane that drying obtains white crystalline powder;
(6) crystalline mother solution utilizes the ion-exchange demineralization technical finesse, crystalline mother solution mixes in 1: 0.5 ratio with pure water, control pH5.5-6.5,35 ℃ of working temperatures, ion exchange column bed length-to-diameter ratio is 6: 1, and the charging flow velocity per hour is that flow is 1.5 times of column volume, returns ceramic membrane membrane filtration process circular treatment again, reclaim product, the inorganic salt of recovery can be done the mineral manure sale also can do the fermention medium batching.
Product tryptophane yield is 99.8%, and the every index of product tryptophane all meets the tryptophane performance index shown in the table 1.
Claims (1)
1. a technology of extracting tryptophane from fermented liquid is characterized in that, may further comprise the steps:
(1) be 30-50g/L with tryptophane, pH value is 4.0-7.0, the residual sugar amount is≤1 times of the tryptophane fermented liquid thin up of 0.5g/L, and fermented liquid is heated to temperature is 50-100 ℃, adopts static mixed technology, and adding concentration is the sulfuric acid of 70-98%, regulate pH to 3-6 by control fermented liquid and vitriolic flow proportional, tryptophane is present in the fermented liquid with solution state, and makes the tropina sex change, be suitable for thalline and separate;
(2) will through the ceramic membrane on-line filtration, remove the whole mycelium in the fermented liquid through step (1) acidifying fermented liquid; Described ceramic membrane membrane pore size is 50nm, and the filtering service temperature of controlling diaphragm is 50-90 ℃, and advancing film pressure is 1.5-3.0bar, filters out the bacterium slag, and the stock liquid volume is concentrated into 8-15 times of bacterium slag volume, and spray is dried can do tropina to the bacterium slag through concentrating;
(3) will remove Deproteinization, macromole impurity and pigment through the rolling organic membrane through the feed liquid behind step (2) filter wash, the described rolling organic membrane molecular weight that dams is 1000, control pH 2.0-5.0, and filtration temperature is 20-40 ℃, controlled filter pressure 10-20bar;
(4) adopt the triple effect falling liquid film to concentrate, 60-90 ℃ of thickening temperature imitated in control one, and 90-110 ℃ of thickening temperature imitated in control two, 50-80 ℃ of control triple effect thickening temperature, the control vacuum pressure be-more than the 0.08Mpa, will be concentrated to state of saturation through the feed liquid after step (3) organic membrane decolours; Then concentrated solution is delivered to the Concentrated and crystallized in vacuum jar immediately, 50-75 ℃ of vacuum concentration temperature, more than vacuum pressure-0.08Mpa, continuing to be concentrated into feed liquid proportion is 1.15-1.4g/cm
3Add ammoniacal liquor then and regulate pH to 4.5-6.8, nature decrease temperature crystalline under the normal pressure, crystallization control process time are 2-6 hour; After crystal was separated out, the new concentrated solution of restock was warmed up to 50-75 ℃ to original volume, and vacuum concentration to feed liquid proportion is 1.15-1.4g/cm
3, ammoniacal liquor is regulated pH to 4.5-6.8, nature decrease temperature crystalline under the normal pressure, and three additional concentrated solutions like this are concentrated into the 30-40% that volume is an original volume at last, obtain sheet tryptophane crystal;
(5) adopt dull and stereotyped centrifuge with cutter discharge of solid to dry and separate the removal crystalline mother solution, collect the tryptophane crystal, it is the product tryptophane that drying obtains white crystalline powder;
(6) crystalline mother solution utilizes macropore cation resin to carry out the desalination processing, crystalline mother solution mixes in 1: 0.5 ratio with pure water, control pH5.5-6.5,35 ℃ of working temperatures, ion exchange column bed length-to-diameter ratio is 6: 1, and the charging flow velocity per hour is 1.5 times of flow column volume, and effluent liquid returns ceramic membrane membrane filtration process circular treatment again, reclaim product, the inorganic salt of wash-out and heteroacid can be done the mineral manure sale also can do the fermention medium batching.
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| JPH0813801B2 (en) * | 1989-06-27 | 1996-02-14 | 三井東圧化学株式会社 | Method for purifying tryptophan |
| CN101531626A (en) * | 2008-03-14 | 2009-09-16 | 江苏诚意药业有限公司 | Refining method for producing L-tryptophan in industrial way by using biofermentation method |
| CN101412716A (en) * | 2008-11-28 | 2009-04-22 | 山东恩贝生物工程有限公司 | Method for extracting lactoflavin |
| CN101456822B (en) * | 2008-11-28 | 2012-07-25 | 山东恩贝生物工程有限公司 | Novel process for extracting threonine |
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