CN101191138A - Method for producing gellan gum finished product from gellan gum fermentation liquor - Google Patents

Method for producing gellan gum finished product from gellan gum fermentation liquor Download PDF

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CN101191138A
CN101191138A CNA2006101188437A CN200610118843A CN101191138A CN 101191138 A CN101191138 A CN 101191138A CN A2006101188437 A CNA2006101188437 A CN A2006101188437A CN 200610118843 A CN200610118843 A CN 200610118843A CN 101191138 A CN101191138 A CN 101191138A
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liquid
obtains
gelling gum
gum
flocculation
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CN101191138B (en
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尹洪波
陈亮
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Zhejiang DSM Zhongken Biotechnology Co Ltd
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Abstract

The invention relates to a method for obtaining transparent hydration inclined gellan gum products from gellan gum fermentation broth, comprising techniques of dehydration and condensation of the fermentation broth, repeated dissolution, clarification, and repeated dehydration and condensation and so on. After the great mass of pigments, residual sugar and metal ions in the fermentation broth are removed by utilizing techniques of condensation and repeated dissolution of the invention, color and transparency of the gellan gum products are improved. The invention can use basically same technological line and production facilities to conveniently and alternately produce low acyl or high acyl gellan gum products according to market demand.

Description

Produce the method for gellan gum finished product from gellan gum fermentation liquid
Technical field
The present invention relates to produce the method for gelling gum goods from gellan gum fermentation liquid.
Background technology
The difference of the gelling gum gel property that causes by acetyl content in the gelling gum polysaccharide molecule; usually the gelling gum product is divided into two kinds: a kind of is the high acyl gellan gum product; easily form viscoelastic gel after the aquation; contained base is a high acyl gellan gum in the normal gellan gum fermentation liquid, the C of the D-glucosyl residue in the repeating unit of its polysaccharide molecule 6Have an appointment and 50% replaced by ethanoyl; Another kind is the low-acyl gellan gum product, by high acyl gellan gum being made the deacylated tRNA base or part deacylated tRNA base obtains, very easily forms the fragility gel after the aquation under cation sites.According to the transparency of solution after the gelling gum aquation, can be divided into transparent gellan gum and nontransparent gelling gum again, contain impurity such as a large amount of bacterial chips, pigment in the nontransparent gelling gum from fermented liquid.The most Application Areas of gelling gum need be dissolved the gelling gum product that the back is transparent, colourless or color and luster is very shallow, is commonly referred to the transparent gellan gum product.
Gelling gum content is very low in the conventional gellan gum fermentation liquid, with the gelling gum polysaccharide in the organic solvent deposit fermented liquids such as alcohol, Crude polysaccharides after the oven dry (or gelling gum crude product) only is the 1.0-2.0% (w/v) of starting fermentation liquid, and wherein impurity such as the thalline in the Crude polysaccharides, albumen accounts for about 50% again.Though gelling gum content is very low, fermentation broth viscosity is very high, can't filter clarification at normal temperatures, and if high temperature filtration in the fermented liquid impurity react to each other to make and darken, thereby be difficult to obtain dissolving transparent, the colourless gelling gum product in back.
CN1351172A disclose a kind of from fermented liquid the technology of low acyl transparent gellangum; the weak point of this technology is: fermented liquid is directly made the deacylated tRNA base handle; the generation brown stain that reacts to each other of some organic matters (as amino acid, sugar, pigment) in high temperature, the high pH bottom fermentation liquid; the reaction solution color is very dark; even later process uses activated carbon decolorizing and micro-filtrate membrane filtration also to be difficult to remove, in addition the filtering cost of high temperature membrane is high, microfiltration membrane high temperature is fragile.
CN1635133A also discloses a kind of method of extracting deacylated gellan gum from fermented liquid; this method also is the fermented liquid that contains a large amount of pigments, fermentation residual sugar directly to be carried out high temperature deacylated tRNA base handle; the acting in conjunction of high temperature and oxygenant has produced more impurity, can only obtain the very dark nontransparent gelling gum of color and luster at last.
CN1687437A discloses a kind of extracting method of high acyl gellan gum, and this method does not have deacylated tRNA base step, but still needs to make pyroprocessing to fermented liquid for sterilization; and owing to the bacterial chip that can't remove in the fermented liquid; product purity is very low, and the dissolving back is muddy, can only be used as low-end product.
So far the report that does not also have transparent type high acyl gellan gum production technology.
Summary of the invention
In view of the weak point of above-mentioned gelling gum extracting method, the purpose of this invention is to provide a kind of method that can obtain high-quality gelling gum in cheap mode, especially obtain the method for the transparent gelling gum product that is easier to aquation.
The inventor discovers, carry out heat or alkaline purification and also can not cause solution colour obviously to be deepened and be easy to filter clarification removing in the fermented liquid gelling gum solution behind the impurity such as most of pigment, residual sugar, salt, proposed elder generation based on this discovery the fermented liquid dehydration is concentrated, carries out after the dissolving again the inventive concept of subsequent technique.
The present invention's design is different from directly carries out high temperature and chemical treatment to obtain the conventional techniques thinking of low-acyl gellan gum when not removing a large amount of impurity of fermented liquid in the state of the art, also abolished the technology prejudice that is difficult to obtain transparent gellan gum, especially transparent high acyl gellan gum with conventional separation means.
Based on above-mentioned discovery and design, the invention provides a kind of method of producing gelling gum from gellan gum fermentation liquid, it comprises technological process:
A. concentration process:
Gellan gum fermentation liquid is made flocculation treatment, solid-liquid separation,, obtain concentrating 5 times or above wet gelling gum crude product to remove most of water and pigment in the fermented liquid;
B. dissolution process again:
The gelling gum crude product that obtains among the A is disperseed again and be dissolved in water, obtain the turbid liquid of gelling gum;
C. clarifying process:
The turbid liquid of gelling gum that obtains among the B is made clarifying treatment, obtain the gelling gum clear liquid;
D. reconcentration process:
The gelling gum clear liquid that obtains among the C is made processed, the gellan gum finished product that obtains wetting;
E. drying and crushing process:
The wet gellan gum finished product that obtains among the D is made dry, pulverization process, obtain gellan gum finished product.
In one embodiment of the invention, flocculation treatment described in the A. concentration process is the metal-salt flocculation, and whole concentration process comprises:
(a) flocculation, add the water-soluble metal salt that 0.2-5.0kg is selected from down the group metal in every 100L fermented liquid: magnesium, calcium, barium, zinc, aluminium or its combination and 0.2-5.0kg are selected from down the alkaline matter of group: potassium hydroxide, sodium hydroxide, salt of wormwood, yellow soda ash or its combination;
(b) solid-liquid separation obtains the gelling gum throw out with the flocculation filtering fermentation liquor dehydration that obtains in (a), wherein is filtered into centrifugal filtration process or pressure filtration method;
(c) desalination comprises: the gelling gum throw out that obtains in (b) is scattered in the low-alcohol solution that is selected from down group: ethanol, Virahol or its combination, and making the determining alcohol in the dispersion liquid is 20-80%; It is acid regulating described dispersion liquid with acid solution; The gelling gum crude product that described dispersion liquid solid-liquid separation is obtained wetting.
In another embodiment of the invention, flocculation treatment described in the A. concentration process is the alcohol flocculation, and whole concentration process comprises:
(a) flocculation adds the alcoholic solution of organizing under being selected from fermented liquid: ethanol, Virahol or its combination, and making the determining alcohol in the flocculation fermented liquid is 30-80% (v/v);
(b) solid-liquid separation is removed the gelling gum crude product that liquid obtains wetting with the filtering fermentation liquor that obtains in (a) flocculating, and wherein is filtered into centrifugal filtration process or pressure filtration method.
In another embodiment of the invention, flocculation treatment described in the A. concentration process is the array mode of metal-salt flocculation and alcohol flocculation, and whole concentration process comprises:
(a) flocculation adds 0.2-5.0kg water-soluble alkali metal salts or alkaline earth salt in every 100L fermented liquid, and adds the alcoholic solution that is selected from down group: ethanol, Virahol or its combination, and making the determining alcohol in the flocculation fermented liquid is 20-50% (v/v);
(b) filter, the flocculation filtering fermentation liquor dehydration that obtains in (a) is obtained the gelling gum throw out, wherein be filtered into centrifuging or pressure filtration;
(c) desalination comprises: the gelling gum throw out that obtains in (b) is scattered in the low-alcohol solution that is selected from down group: ethanol, Virahol or its combination, and making the determining alcohol in the dispersion liquid is 20-80%; Described dispersion liquid is removed by filter the gelling gum crude product that liquid obtains wetting.
In the dissolution process, the turbid liquid of gelling gum is long-pending to be initial 0.2-1.2 times of fermentating liquid volume of described gelling gum crude product institute correspondence.
In the specific embodiment of the present invention, the clarification mode in the C. clarifying process of the present invention is selected from down group: sheet frame or van-type press filtration, vacuum filtration, or centrifugal clarification.
In one embodiment of the present invention, the dewatering type of D. reconcentration process is the gel evaporation, and described reconcentration process comprises:
(a) gel adds gelating agent in the gelling gum clear liquid that obtains in C, form gel, and wherein said gelating agent is an an alkali metal salt, and consumption is the 0.2-5.0% (w/v) of glue;
(b) dehydration dewaters the gellan gum finished product that obtains wetting with the gel squeezing that obtains in (a).
In the another embodiment of the invention, the dewatering type of D. reconcentration process is the pure precipitator method, and described reconcentration process comprises:
(a) precipitation adds the alcoholic solution that is selected from down group in the gelling gum clear liquid that obtains in C: ethanol, Virahol or its combination, and making the determining alcohol in the gained precipitated liquid is 40-80% (v/v);
(b) dehydration is removed liquid, the gellan gum finished product that obtains wetting with the precipitated liquid that obtains in (a) through centrifugal or squeezing.
In another embodiment of the present invention, the dewatering type of D. reconcentration process is an alkoxide co-coagulation mode, and described reconcentration process comprises:
(a) add water-soluble alkali metal salts in the gelling gum clear liquid that obtains in C, consumption is the 0.2-5.0% (w/v) of glue, and adds the alcoholic solution that is selected from down group: ethanol, Virahol or its combination, and making the determining alcohol in the gained precipitated liquid is 30-60% (v/v);
(b) precipitated liquid of (a) is squeezed or the centrifugal liquid of removing the gellan gum finished product that obtains wetting.
For obtaining the low-acyl gellan gum product, in a kind of embodiment of invention, gelling gum solution is carried out the deacylated tRNA base handle, described gelling gum solution is to obtain the gelling gum clear liquid among the turbid liquid of gelling gum that obtains among the B or the C.Preferably, the turbid liquid of gelling gum that obtains in to B before the C. clarifying process begins carries out the deacylated tRNA base and handles.
The advantage of the inventive method is:
1, dehydration concentrates and to remove in the fermented liquid after most pigment, residual sugar, the salt, and the dissolved gelling gum is difficult for brown stain through high temperature filtration or high temperature alkaline purification again, thereby improves the color and luster of gelling gum product, and the easier aquation of low product salt.
2, need not the clarifying effect that micro-filtrate membrane filtration also can obtain.Because behind the fermented liquid flocculation dewatering, also removed the most of metal-salt in the substratum, soltion viscosity descends under the low metal ion concentration, be beneficial to filtration, centrifugally operated, and dissolved gelling gum solution is in the low ion concns environment and makes greater protein matter be in particulate state flocculation state again, need not micro-filtration and also can easily remove, and the gelling gum product protein content that obtains is few by the clarification mode of routine, more transparent after the aquation.
3, can alternately produce transparent low acyl group or high acyl gellan gum product according to the market requirement easily with essentially identical operational path and production unit, but before the present invention, also not have the transparent type high acyl gellan gum products production technology of bibliographical information industrialization.
4, except that above-mentioned advantage, if A concentration process of the inventive method and D reconcentration process adopt metal-salt flocculence, gel evaporation respectively, can significantly reduce the consumption of alcohol, make low production cost.
Embodiment
Method of producing gelling gum provided by the invention from gellan gum fermentation liquid, it comprises:
A. concentration process: gellan gum fermentation liquid is made flocculation treatment, solid-liquid separation,, obtain concentrating 5 times or above wet gelling gum crude product to remove most of water and pigment in the fermented liquid;
B. dissolution process again: the gelling gum crude product that obtains among the A is disperseed again and be dissolved in water, obtain the turbid liquid of gelling gum;
C. clarifying process: the turbid liquid of gelling gum that obtains among the B is made clarifying treatment, obtain the gelling gum clear liquid;
D. reconcentration process: the gelling gum clear liquid that obtains among the C is made processed, the gellan gum finished product that obtains wetting;
E. drying and crushing process: the wet gellan gum finished product that obtains among the D is made dry, pulverization process, obtain gellan gum finished product.
The flocculation treatment of the A. concentration process of the inventive method can adopt organic solvent flocculence commonly used in the polysaccharide extraction, salt flocculence, tensio-active agent flocculence etc.Preferably, adopt pure flocculence or metal-salt flocculence.
Gelling gum is an electronegativity, can gel under cation sites or gathering, and monovalence, divalence or trivalent metal ion all can work, and better effects if under the alkaline condition, easy flocculation dewatering.
When adopting the metal-salt flocculence, in a kind of embodiment of the inventive method, the A. concentration process comprises: (a) flocculation.Add the soluble metallic salt that is selected from down group in fermented liquid: magnesium, calcium, barium, zinc, aluminium or its combination, consumption are to add above-mentioned water-soluble metal salt 0.2-5.0kg in every 100L fermented liquid, stir evenly.Preferable metal-salt is the soluble salt of magnesium, calcium, aluminium, better is the muriate of magnesium, calcium, aluminium, preferable consumption is the 0.5-3.0kg/100L fermented liquid, better is the 1.0-2.0kg/100L fermented liquid, metal-salt can solid or the solution form add, the present invention preferably uses the solution form to add.And in fermented liquid, add alkaline matter, flocculate to fermented liquid, in the specific embodiment of the present invention, the consumption that adds 0.2-5.0kg with every 100L fermented liquid adds the alkaline matter that is selected from down group to fermented liquid: potassium hydroxide, sodium hydroxide, salt of wormwood, yellow soda ash or its combination stir evenly.Preferred alkaline matter is potassium hydroxide, sodium hydroxide, and preferable consumption is 0.5-3.0kg, and that better is 1.0-2.0kg/100L, preferably adds with the solution form.(b) solid-liquid separation.The flocculation fermented liquid dehydration that obtains in (a) is obtained the gelling gum throw out, conventional solid-liquid separating method all can be used for the present invention, the preferred centrifugal filtration process that uses, as the cloth bag that utilizes tripod pendulum type batch centrifugal is centrifugal dewaters, or the pressure filtration method, as plate and frame or van-type press filtration, screw extrusion/squeeze and filter etc.Usually, the gelling gum throw out that obtains of dehydration be initial fermented liquid 20% (w/v) or below, promptly concentrate 5 times or more than, preferably, concentrate 8 times or higher, this step can be sloughed partial pigment, the residual sugar in the fermented liquid.(c) desalination.Purpose is metal-salt residual that sloughs the adding in (a), and further sloughs pigment, residual sugar etc., makes the easier aquation of product, whiter, more transparent.This step comprises: the gelling gum throw out that obtains in (b) is scattered in the low-alcohol solution that is selected from down group: ethanol, Virahol or its combination, but the lower alcohol of C1-C4 all is fit to the present invention, making the determining alcohol in the dispersion liquid is 20-80% (v/v), and that preferable is 30-60%; It is acid regulating described dispersion liquid with acid solution, as being 2.0-6.5 with sulfuric acid, hydrochloric acid or adjusting pH, is preferably pH 2.0-5.0; Described dispersion liquid is removed the gelling gum crude product that liquid obtains wetting with the method for above-mentioned solid-liquid separation, this gelling gum crude product contains gelling gum polysaccharide, bacterial chip and alcohol and water, its total amount is below 20% (w/v) of initial fermented liquid, promptly concentrate about more than 5 times, preferably should concentrate 8 times or more than, more preferably be 15 times or more than, better is 15-30 is doubly.
Concentration process of the present invention also can adopt pure flocculence, and the A. concentration process comprises: (a) flocculation.It is 30-80% (v/v) that the low-alcohol solution that adds C1-C4 in fermented liquid makes the determining alcohol in the fermented liquid that flocculates, the preferred alcoholic solution that is selected from down group that uses: ethanol, Virahol or its combination.Take all factors into consideration cost and effect, preferable consumption is 40-60% (v/v); Mixing.(b) solid-liquid separation.With solid-liquid separating method used in the above-mentioned metal-salt flocculence fermented liquid that obtains flocculating in (a) is removed liquid, obtain removing the wet gelling gum crude product of the most of pigment of fermented liquid, residual sugar, salinity, this gelling gum crude product contains gelling gum polysaccharide, bacterial chip and alcohol and water, its total amount be initial fermented liquid 12% (w/v) or below, promptly concentrate about 5 times or more than, preferably be 8 times, more preferably be 15 times or more than, better is 15-30 is doubly.
Metal-salt flocculence cost is low, and pure flocculence uses more convenient, and for making up both advantages, in another embodiment of the invention, flocculation treatment described in the A. concentration process is an alkoxide co-coagulation mode, and whole concentration process comprises: (a) flocculation.Add 0.2-5.0kg water-soluble alkali metal salts or water-soluble alkali earth metal salt in every 100L fermented liquid, preferable consumption is 0.5-2.0kg; And the low-alcohol solution of adding C1-C4, be preferably the alcoholic solution that is selected from down group: ethanol, Virahol or its combination, making the determining alcohol in the flocculation fermented liquid is 20-50% (v/v), is preferably 30-40%.(b) filter.The flocculation fermented liquid solid-liquid separation that obtains in (a) is obtained the gelling gum throw out.(c) desalination.Comprise: the gelling gum throw out that obtains in (b) is scattered in the low-alcohol solution that is selected from down group: ethanol, Virahol or its combination, making the determining alcohol in the dispersion liquid is 20-80%, is adjusted to acidity with acid solution; Described dispersion liquid is removed by filter the gelling gum crude product that liquid obtains wetting.
As possibility, when finishing, the A. concentration process increases washing operation again, and comprise and the gelling gum crude product disperseed or be soaked in organic solvent, washing, solid-liquid separation such as alcohol, make the gelling gum crude product color that obtains more shallow.
The B. of the inventive method dissolution process again is mainly clarifying process and prepares, its main points are that gelling gum concentration should be higher, make that the subsequent operations volume is little, cost is low, but gelling gum is fully dissolved to improve yield, to keep solution to be difficult for gel or modest viscosity is easily clarified.Usually, the turbid liquid of gelling gum amasss 0.2-1.2 times for the corresponding initial fermentating liquid volume of used gelling gum crude product, it preferably is 0.4-0.8 times, promptly concentrate 1.2-2.5 doubly, solvent temperature is generally 70-95 ℃, usually can obviously see the tiny flocculation particle that is formed by bacterial chip, albumen etc. in the solution, this helps obtaining very transparent clear liquid.This technology also plays the purpose that substitutes the fermented liquid sterilization simultaneously.
The C. clarifying process of the inventive method is in order to remove the impurity such as bacterial chip in the turbid liquid of gelling gum, the liquid defecation method that biological technical field is commonly used all can use, as sheet frame or van-type press filtration, vacuum filtration or centrifugal clarification, use flocculating aids can improve filter effect when press filtration or vacuum filtration.Certainly also can use micro-filtrate membrane filtration, but cost is too high.All should keep not gel or be easy to filter than low viscosity and wait clarification to operate of gelling gum solution when adopting above-mentioned clarification mode, need remain on usually 60 ℃ or more than.In the resulting gelling gum clear liquid, the gelling gum content behind the impurity such as removal bacterial chip is 0.5-3.0% (w/v), and preferable content is 0.8-2.0% (w/v).
The D. reconcentration process of the inventive method is to reclaim the gelling gum of purifying to obtain finished product.Organic solvent precipitation method, gel evaporation, dehydration by evaporation method or membrane concentration method etc. all can be used for the present invention.
In a kind of embodiment of the present invention, the characteristic of utilizing gelling gum to meet the cation easily gel adopts metal-salt gel evaporation, and the 1-3 valence metal ion all can use, and preferably uses monovalent metallic ion, and described reconcentration process comprises: (a) gel.Add gelating agent in the gelling gum clear liquid that in technological process C, obtains, form gel, wherein said gelating agent is an an alkali metal salt, consumption is the 0.2-5.0% (w/v) of glue, preferable gelating agent is the salt of potassium or sodium, better is sodium-chlor or Repone K, and preferable consumption is 0.5-3.0% (w/v), and that better is 0.8-2.0% (w/v).(b) dehydration.The gel squeezing that obtains in (a) is dewatered the gellan gum finished product that obtains wetting.Gel squeezing dewaters and comprises: the cloth bag squeezing dewaters, sheet frame or box filter filter-press dehydration, diaphragm pressing type pressure filter filter-press dehydration or the like.The gellan gum finished product that obtains is generally half-dried gelling gum blob of viscose or film.
In a kind of embodiment of the present invention, the dewatering type of D. reconcentration process is the machine solvent precipitation, the especially pure precipitator method, and described reconcentration process comprises: (a) precipitation.The low-alcohol solution of C1-C4 in the gelling gum clear liquid that obtains in C, the preferred alcoholic solution that is selected from down group that adds: ethanol, Virahol or its combination, making the determining alcohol in the gained precipitated liquid is 40-80% (v/v), is preferably 50-70% (v/v), mixing.(b) dehydration.The precipitated liquid that obtains in (a) is removed liquid through centrifugal or squeezing, and the gellan gum finished product that obtains wetting is cotton-shaped, bulk or sheet usually.Describedly centrifugally comprise common 3-foot centrifuge dehydration, the spiral shell discharging of crouching is centrifugal, described squeezing comprises: the cloth bag squeezing dewaters, sheet frame or box filter filter-press dehydration, diaphragm pressing type pressure filter filter-press dehydration or the like.
In the another embodiment of the present invention, D. the dewatering type of reconcentration process is the combination of the pure precipitator method and gel evaporation, described reconcentration process comprises: add an alkali metal salt in the gelling gum clear liquid that (a) obtains in C, consumption is the 0.5-3.0% (w/v) of glue, preferably, add sylvite or sodium salt, consumption is 0.2-5.0% (w/v), preferable consumption is 0.5-2.0% (w/v), and the low-alcohol solution of adding C1-C4, the preferred alcoholic solution that is selected from down group that adds: ethanol, Virahol or its combination, making the determining alcohol in the gained precipitated liquid is 30-60% (v/v), is preferably 40-60% (v/v).(b) precipitated liquid of (a) is squeezed or the centrifugal liquid of removing the gellan gum finished product that obtains wetting.
Metal-salt used herein can solid or the form of solution add.
The turbid liquid of gelling gum that is used for C. clarifying process of the present invention can be to handle through the deacylated tRNA base, also can handle without the deacylated tRNA base.
The gelling gum clear liquid that is used for D. reconcentration process of the present invention can be to handle through the deacylated tRNA base, also can handle without the deacylated tRNA base.
For obtaining the low-acyl gellan gum product, in a kind of embodiment of invention, the turbid liquid of gelling gum that obtains in to B. the C. clarifying process begins before carries out the processing of deacylated tRNA base.Described deacylated tRNA base is handled and is comprised alkaline purification commonly used in the prior art, other deacetylation reaction that also can use organic chemistry filed to use always.
The wet gellan gum finished product that dehydration is obtained can carry out processing such as stripping and slicing/sheet, granulation before dry, drying and breaking method that food and biological technical field are commonly used all can be used for the present invention.Drying commonly used is convection oven drying, vacuum-drying, fluidized drying etc.Gelling gum product after drying and the pulverizing is generally white or oyster white, transparent or substantially transparent after the aquation.
Numerous documents such as CN1351172A and CN1635132A all disclose the method for fermentative Production gelling gum.The gellan gum fermentation liquid that contains arbitrarily normal gelling gum content all can be used for implementing the inventive method, fermented liquid commonly used is the gellan gum fermentation liquid of waterweed pseudomonas (Pseudomonas elodea), and used fermented liquid can be earlier through germicidal treatment or without germicidal treatment.In order to reduce pigment in the fermented liquid to the influence of quality product, preferred sucrose and the dregs of beans used is respectively as the main carbon, the nitrogenous source that ferment in fermentation, because main carbon source commonly used such as glucose or amylum hydrolysate of the sugar be easily brown stain at high temperature, major nitrogen source such as yeast extract paste/powder, fish meal etc. commonly used not only make the fermented liquid color burn, and peculiar smell is arranged.
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.In addition, unless stated otherwise, otherwise all relate to concentration per-cent all be weight/volume (w/v) per-cent.
Raw material: gellan gum fermentation liquid.The gelling gum content in crude product is 1.8g/100ml (1.8%) in the fermented liquid with recording after alcohol precipitation, the drying.
Embodiment 1
A. concentration process
1. in the flocculation jar that the 10m3 fermented liquid is housed, under the normal temperature, add the about 250L of 20% Adlerika, add 40% sodium hydroxide solution 500L while stirring, obtain the fermented liquid that flocculates.
2. deliver to the plate-and-frame filter press filter dehydration with the pump fermented liquid that will flocculate, and wash with the clear water top, discharging obtains 2000kg gelling gum throw out.
3. the gelling gum throw out is dosed to the desalination washing tank, the about 1m3 of aqueous isopropanol that adds 90% (v/v), dispersed with stirring, isopropyl alcohol concentration is about 50% (v/v) in the dispersion liquid, transferring pH with hydrochloric acid is about 5.0, take off liquid with the tripod pendulum type batch centrifugal filtration behind about 60min, obtain about 1200kg gelling gum crude product.
B. dissolution process again
4. add the about 5m3 of water in the glue pot, be warming up to 80 ℃, add whole above-mentioned gelling gum crude products, stirring and dissolving obtains the turbid liquid of gelling gum.
C. clarifying process
5. while hot with the turbid liquid of the plate and frame(type)filter press filtration above-mentioned gelling gum of clarification of precoating super-cell, obtain about 5.5m3 gelling gum clear liquid, insert setting tank.
D. reconcentration process
6. the gelling gum clear liquid in the above-mentioned setting tank is cooled to below 50 ℃, adds the about 10m3 of 95% (v/v) ethanolic soln, mixing obtains the gelling gum precipitation, takes off liquid with the spiral shell discharging formula whizzer that crouches and obtains the wet gellan gum finished product of about 200kg.
E. drying and crushing
7. dry above-mentioned wet product with the blowing-type loft drier, obtain the Powdered gellan gum finished product of about 95kg after pulverizing with beater grinder.Product is the high acyl gellan gum product, is designated as 1-HA.
Embodiment 2
A. concentration process
1. in the flocculation jar that the 10m3 fermented liquid is housed, add the about 15m3 of 98% (v/v) Virahol, stir, obtain the flocculation fermented liquid.
2. deliver to plate-and-frame filter press and filter and to take off liquid with the pump fermented liquid that will flocculate.
3. wash the back discharging with a small amount of Virahol top, obtain the wet gelling gum crude product of 700kg.
B. dissolution process again
4. add the about 3.5m3 of water in the glue pot, be warming up to 80 ℃, add whole above-mentioned gelling gum crude products, stirring and dissolving obtains the turbid liquid of gelling gum.
4a. alkaline purification: adding alkali lye while hot in the turbid liquid of gelling gum, to make glue pH be 9.5-10.5, keeps about 10min, with acid solution pH is lowered to 6.0-8.0 again.
C. clarifying process
5. while hot with the turbid liquid of the vacuum drum machine filtration above-mentioned gelling gum of clarification of precoating super-cell, obtain about 4m3 gelling gum clear liquid, insert setting tank.
D. reconcentration process
6. the gelling gum clear liquid in the above-mentioned setting tank is cooled to about 50 ℃, adds 20% sodium chloride solution 400L, mixing, cooling obtains the gelling gum gel, is sub-packed in the cloth bag that industrial filter cloth is made, and obtains the wet gellan gum finished product of 300kg with the oil press squeezing.
E. drying and crushing
7. dry above-mentioned wet product with the blowing-type loft drier, obtain the Powdered gellan gum finished product of about 95kg after pulverizing with beater grinder.Product is the low-acyl gellan gum product, is designated as 2-LA.
Embodiment 3
The method of reference example 1, difference are step 1-3:
1. in the flocculation jar that the 10m3 fermented liquid is housed, add the about 10m3 of 95% (v/v) ethanol, stir, obtain the fermented liquid that flocculates.
2. deliver to plate-and-frame filter press and filter and to take off liquid with the pump fermented liquid that will flocculate, discharging obtains the wet gelling gum crude product of 1200kg.
3. the gelling gum crude product is dosed to washing tank, adds the about 500L of ethanolic soln of 90% (v/v), dispersed with stirring is filtered with tripod pendulum type batch centrifugal then and is taken off liquid, obtains about 700kg gelling gum crude product.Product is the high acyl gellan gum product, is designated as 3-HA.
Embodiment 4
The method of reference example 1, difference is step 1:
1. in the flocculation jar that the 10m3 fermented liquid is housed, add the about 750L of 40% calcium chloride solution, add 40% potassium hydroxide solution 125L while stirring, obtain the fermented liquid that flocculates.
Product is the high acyl gellan gum product, is designated as 4-HA.
Embodiment 5
The method of reference implementation 1, difference are following step 1:
1. in the flocculation jar that the 10m3 fermented liquid is housed, add the about 500L of 20% liquor alumini chloridi, add 40% potassium hydroxide solution 250L while stirring, obtain the fermented liquid that flocculates.
Product is the high acyl gellan gum product, is designated as 5-HA.
Embodiment 6
The method of reference example 2, difference are step 1-3:
1. in the flocculation jar that the 10m3 fermented liquid is housed, add the about 500L of 20% liquor zinci chloridi, add 40% sodium carbonate solution 500L while stirring, obtain the fermented liquid that flocculates.
2. deliver to the plate-and-frame filter press filter dehydration with the pump fermented liquid that will flocculate, and wash with the clear water top, discharging obtains 1200kg gelling gum throw out.
3. the gelling gum throw out is dosed to the desalination washing tank, the about 1000L of ethanolic soln that adds 90% (v/v), dispersed with stirring, alcohol concn is about 50% (v/v) in the dispersion liquid, transferring pH with hydrochloric acid is about 5.0, take off liquid with the tripod pendulum type batch centrifugal filtration after keeping about 10min, obtain about 500kg gelling gum crude product.
Product is the low-acyl gellan gum product, is designated as 6-LA.
Embodiment 7
The method of reference example 6, difference is step 1:
1. in the flocculation jar that the 10m3 fermented liquid is housed, add the about 700L of 30% calcium chloride solution, add 10% sodium hydroxide solution 500L while stirring, obtain the fermented liquid that flocculates.
Product is the low-acyl gellan gum product, is designated as 7-LA.
Embodiment 8
Method with reference to 6, not middle part is step 6:
6. the gelling gum clear liquid in the above-mentioned setting tank is cooled to below 50 ℃, adds the about 10m3 of aqueous isopropanol of 98% (v/v), mixing obtains the gelling gum precipitation, takes off liquid with the spiral shell conveyer centrifugal that crouches and obtains the wet gellan gum finished product of about 150kg.
Product is the low-acyl gellan gum product, is designated as 8-LA.
Reference examples 1 (fermented liquid High Temperature Sterilization, flocculation dewatering prepare opaque high acyl gellan gum)
1. fermentation liquor pretreatment: fermented liquid is transferred pH value 4-4.5, heat up 90 ± 2 ℃, the enzyme that goes out kills thalline, keeps 30min.
2. flocculating settling: add 10% calcium chloride solution that accounts for fermentating liquid volume 2% to pretreated fermented liquid, add fermentating liquid volume 30%, concentration is to stir behind 95% the Virahol.
3. solid-liquid separation: the spiral shell conveyer centrifugal that crouches takes off liquid and obtains gelling gum crude product throw out.
4. dry, pulverizing: vacuum-drying, pulverize the gelling gum powder-product.Product is the high acyl gellan gum product, is designated as C-HA.
Reference examples 2 (the direct deacylated tRNA base processing of fermented liquid, micro-filtrate membrane filtration clarification preparation low-acyl gellan gum)
A. deacylated tRNA base technology
1. the 500L fermented liquid is heated to 90 ℃; Transfer pH to 10 with NaOH, be incubated 85 ℃-90 ℃, 15 minutes; Transfer pH to 6-8 with dilute hydrochloric acid.
B. clarification process
2. coarse filtration.The diatomite that adds fermentating liquid volume 1%, 0.2% gac, by filtering through the diatomaceous plate-and-frame filter press of precoating, pressure is 0.2-0.3Mpa, the temperature for the treatment of filtrate is 80-90 ℃.
3. micro-filtration.The filtrate that coarse filtration gets is micro-filtration (temperature is greater than 70 ℃) while hot, uses ceramic microfiltration membrane to carry out.
C. gel dewatering process
4. constantly stir the sodium chloride solution that in hot filtrate, slowly adds 50L 20% down, be cooled to room temperature and form gel.
5. gel piece is smashed in the bag that the filter cloth of packing into makes, tying places the fluid press under and squeezed 2 hours.
D. drying and pulverizing
6. with 60 ℃ of oven dry of half-dried film 3 hours, pulverize and be finished product.Product is the low-acyl gellan gum product, is designated as C-LA.
The result relatively
Table 1 high acyl gellan gum product relatively
Figure A20061011884300141
Table 2 low-acyl gellan gum product relatively
Figure A20061011884300142
The front elaborates and illustrates the present invention's skill process that respectively struggles against, but should understand, these explanations are in order to help those skilled in the art to understand better and to implement the present invention, main points of the present invention and creativeness are mainly to have adopted that gelling gum dehydration concentrates, the spissated operational path that dewaters again after the dissolving, clarification, but not the detail parameters of each technological process.
Every piece of document quoting in this paper is all included this paper in as a reference.In addition, should be understood that read of the present invention above-mentioned tell about content after, those skilled in the art can make various changes or modifications the present invention, these equivalent form of values fall within the application's appended claims institute restricted portion equally.

Claims (10)

1. method of producing the transparent gellan gum product from gellan gum fermentation liquid, it comprises technological process:
A. concentration process:
Gellan gum fermentation liquid is made flocculation treatment, solid-liquid separation, to remove most of water, pigment and salt in the fermented liquid, obtain concentrating 5 times or above wet gelling gum crude product, wherein said flocculation mode is selected from: alcohol flocculation, salt flocculation or alkoxide co-coagulation mode;
B. dissolution process again:
The gelling gum crude product that obtains among the A is disperseed again and be dissolved in water, obtain the turbid liquid of gelling gum;
C. clarifying process:
The turbid liquid of gelling gum that obtains among the B is made clarifying treatment, obtain the gelling gum clear liquid;
D. reconcentration process:
The gelling gum clear liquid that obtains among the C is made processed, the gellan gum finished product that obtains wetting, wherein said dewatering type is selected from: the pure precipitator method, gel evaporation or its array mode;
E. drying and crushing process:
The wet gellan gum finished product that obtains among the D is made dry, pulverization process, obtain gellan gum finished product.
2. the method for claim 1 is characterized in that, flocculation treatment described in the A. concentration process is the metal-salt flocculation, and concentration process comprises:
(a) flocculation, add the water-soluble metal salt that 0.2-5.0kg is selected from down the group metal in every 100L fermented liquid: magnesium, calcium, barium, zinc, aluminium or its combination and 0.2-5.0kg are selected from down the alkaline matter of group: potassium hydroxide, sodium hydroxide, salt of wormwood, yellow soda ash or its combination;
(b) solid-liquid separation obtains the gelling gum throw out with the flocculation filtering fermentation liquor dehydration that obtains in (a), wherein is filtered into centrifugal filtration process or pressure filtration method;
(c) desalination comprises: the gelling gum throw out that obtains in (b) is scattered in the low-alcohol solution that is selected from down group: ethanol, Virahol or its combination, and making the determining alcohol in the dispersion liquid is 20-80%; It is acid regulating described dispersion liquid with acid solution; The gelling gum crude product that described dispersion liquid solid-liquid separation is obtained wetting.
3. the method for claim 1 is characterized in that, flocculation treatment described in the A. concentration process is the alcohol flocculation, and concentration process comprises:
(a) flocculation adds the alcoholic solution of organizing under being selected from fermented liquid: ethanol, Virahol or its combination, and making the determining alcohol in the flocculation fermented liquid is 30-80% (v/v);
(b) solid-liquid separation is removed the gelling gum crude product that liquid obtains wetting with the filtering fermentation liquor that obtains in (a) flocculating,
Wherein be filtered into centrifugal filtration process or pressure filtration method.
4. the method for claim 1 is characterized in that, the clarification mode in the C. clarifying process is selected from down group: sheet frame or van-type press filtration, vacuum filtration, or centrifugal clarification.
5. the method for claim 1 is characterized in that, the dewatering type of D. reconcentration process is the gel evaporation, and the reconcentration process comprises:
(a) gel adds gelating agent in the gelling gum clear liquid that obtains in C, form gel, and wherein said gelating agent is a water-soluble alkali metal salts, and consumption is the 0.2-5.0% (w/v) of glue;
(b) dehydration dewaters the gellan gum finished product that obtains wetting with the gel squeezing that obtains in (a).
6. the method for claim 1 is characterized in that, the dewatering type of D. reconcentration process is the pure precipitator method, and the reconcentration process comprises:
(a) precipitation adds the alcoholic solution that is selected from down group in the gelling gum clear liquid that obtains in C: ethanol, Virahol or its combination, and making the determining alcohol in the gained precipitated liquid is 40-80% (v/v);
(b) dehydration is removed liquid, the gellan gum finished product that obtains wetting with the precipitated liquid that obtains in (a) through centrifugal or squeezing.
7. the method described in claim 1 is characterized in that, the dewatering type of D. reconcentration process is the array mode of the pure precipitator method and gel evaporation, and the reconcentration process comprises:
(a) add an alkali metal salt in the gelling gum clear liquid that obtains in C, consumption is the 0.2-5.0% (w/v) of glue, and adds the alcoholic solution that is selected from down group: ethanol, Virahol or its combination, and making the determining alcohol in the gained precipitated liquid is 30-60% (v/v);
(b) precipitated liquid of (a) is squeezed or the centrifugal liquid of removing the gellan gum finished product that obtains wetting.
8. as claim 1, each described method is characterized in that among the 4-7, and flocculation treatment described in the A. concentration process is an alkoxide co-coagulation mode, and concentration process comprises:
(a) flocculation adds 0.2-5.0kg water-soluble alkali metal salts or alkaline earth salt in every 100L fermented liquid, and adds the alcoholic solution that is selected from down group: ethanol, Virahol or its combination, and making the determining alcohol in the flocculation fermented liquid is 20-50% (v/v);
(b) filter, the flocculation filtering fermentation liquor dehydration that obtains in (a) is obtained the gelling gum throw out, wherein be filtered into centrifuging or pressure filtration;
(c) desalination comprises: the gelling gum throw out that obtains in (b) is scattered in the low-alcohol solution that is selected from down group: ethanol, Virahol or its combination, and the determining alcohol that makes dispersion liquid is 20-80%; It is acid regulating described dispersion liquid with acid solution; Described dispersion liquid is removed by filter the gelling gum crude product that liquid obtains wetting.
9. as each described method among the claim 1-7, it is characterized in that, gelling gum solution carried out the deacylated tRNA base handle that described gelling gum solution is to obtain the gelling gum clear liquid among the turbid liquid of gelling gum that obtains among the B or the C.
10. method as claimed in claim 8 is characterized in that, the turbid liquid of gelling gum that obtains in to B before the C. clarifying process begins carries out the deacylated tRNA base to be handled.
CN2006101188437A 2006-11-28 2006-11-28 Method for producing gellan gum finished product from gellan gum fermentation liquor Expired - Fee Related CN101191138B (en)

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