CN101824095B - Transparent high acyl gellan gum and production method thereof - Google Patents
Transparent high acyl gellan gum and production method thereof Download PDFInfo
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- CN101824095B CN101824095B CN200910052217A CN200910052217A CN101824095B CN 101824095 B CN101824095 B CN 101824095B CN 200910052217 A CN200910052217 A CN 200910052217A CN 200910052217 A CN200910052217 A CN 200910052217A CN 101824095 B CN101824095 B CN 101824095B
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Abstract
The invention relates to a transparent high acyl gellan gum and a production method thereof. The method comprises the following steps: a. carrying out flocculation treatment on gum fermentation liquor with inorganic acid and lower alcohol gellan; b. dehydrating the flocculation material; c. adding water to the dehydrated flocculation material for re-dissolution; d. regulating pH value to 6-7 with inorganic base; e. adding a decolorizer to the gum solution for decoloration and then filtering; f. carrying out flocculation treatment on filter liquor and re-dehydrating; and g. drying to obtain finished product. Compared with the prior art, the invention has the advantages that processing steps are simplified, product quality is improved, production cost is lowed, and waste residue/waste water/waste gas emission is reduced.
Description
Technical field
The present invention relates to the production field of microbiological polysaccharide Gellan gum, more specifically, the present invention relates to transparent high acyl gellan gum and preparation method thereof.
Background technology
Obtaining the gelling gum that drugs approved by FDA is used in 1992, is a kind of high-quality gelifying agent and suspension agent, has using value in foodstuff additive, pharmaceutical excipient and fields such as mikrobe and plant tissue culture media.
China uses as foodstuff additive in approval gelling gum in 1996, in recent years, begins to increase gradually in the application of food service industry gelling gum as a kind of high-grade gelifying agent and suspension agent.
00125858.3 (the applying date of one Chinese patent application CN; On October 26th, 2000) a kind of microbiological polysaccharide Gellan gum production technique is disclosed.
Usually, according to the difference of some compositions in the molecular structure, the gelling gum product is divided into two kinds.
A kind of gelling gum is to slough low acyl group or deacylated gellan gum behind most of ethanoyl through the method for alkaline purification under the high temperature.Such gelling gum has fabulous gelation.Impurity such as the thalline that in leaching process, fermented liquid is brought, pigment are removed, and can obtain the transparent gellan gum of deacylated tRNA base.
The C of the D-glucosyl residue in the repeating unit of another kind of gelling gum polysaccharide molecule
6Have an appointment 50% by the ethanoyl replacement, have the effect that hinders molecule structure of an essay net formation gel, thereby have good visco-elasticity, be referred to as high acyl gellan gum.Because the gelling gum in the fermented liquid promptly is this type, claims natural gelling gum again.High acyl gellan gum is applied to industry such as food, medicine, is a kind of novel additive.CP-Kelco company realized industrialization in 1998.Its colloidal soft and flexible, can be used in dairy products, sauces, jams, jelly, beverages, candy, pudding, etc., giving them a unique flavor.
In addition, according to the transparency of solution after the gelling gum aquation, can gelling gum be divided into transparent type and nontransparent type gelling gum.
The high acyl gellan gum commodity of producing at present are non-transparent types, and its gel purity is low, is milky muddy thing, and its quality and range of application are restricted.
CN101191138A discloses a kind of high acyl gellan gum preparation technology of transparent type, but has the desalination link in the process step, influences quality product, and cost is high, and three waste discharge is high.Particularly, CN101191138A adopts salt flocculation or alkoxide co-coagulation mode, and the consumption of salt reaches the 0.2%-5% of fermented liquid, and the consumption of alkali is 0.2%-5%, and has increased desalinating process one, consumes the water of 20%-80% more.The document also discloses that the embodiment that uses pure flocculence.Yet as flucculation process the earliest, its shortcoming is that pure consumption is very big.For example in the embodiment 2 of the document, for the Virahol of 15 cubic metre 98% of 10 cubic metres of fermented liquids interpolation; In embodiment 3,10 cubic metres of fermented liquids are added 10 cubic metre 95% ethanol, pure consumption is very big.
Adopt activated carbon to make sorbent material among the CN1635133A, clean yet exist the filter cloth bag to be difficult to washing in process of production, and the shortcoming of easy polluted product.
In sum, it is easy that this area presses for development technology, the working method of the production transparent high acyl gellan gum that environmental pollution is little.
Summary of the invention
It is easy that the object of the invention just provides a kind of technology, the working method of the production transparent high acyl gellan gum that environmental pollution is little.
In first aspect of the present invention, a kind of method for preparing the transparent type high acyl gellan gum is provided, described method comprises step:
A. gellan gum fermentation liquid is mixed with mineral acid and lower alcohol and carry out flocculation treatment, thereby obtain to contain the flocculation material of gelling gum throw out;
B. described flocculation material is dewatered, obtain the flocculation material of dehydration;
C. the flocculation material (like filter cake) that dewaters is added entry and dissolve again, thereby acquisition contains the glue of gelling gum;
D. regulate the pH to 6-7 of the glue of said gelling gum with mineral alkali;
E. the adding discoloring agent decolours and filters in said glue, obtains to contain the filtrating of gelling gum;
F. the said filtrating that contains gelling gum is carried out flocculation treatment, and dehydration once more, the wet article of gelling gum that dewater obtained; With
G. the wet article of described gelling gum are carried out drying, obtain transparent type high acyl gellan gum product.
In another kind of preference, in said step a, mineral acid is selected from down group: hydrochloric acid, sulfuric acid or its combination.
In another kind of preference, the concentration of mineral acid is 1-5wt%.
In another kind of preference, in said step a, regulate the pH to 1.0-3.5 of fermented liquid with mineral acid.
In another kind of preference, regulate the pH to 1.5-2.5 (acidity of the liquid that promptly flocculates is pH 1.5-2.5) of fermented liquid with mineral acid.
In another kind of preference, in said step a, lower alcohol is selected from down group: ethanol, Virahol, or its combination.
In another kind of preference, in said step a, in fermented liquid, do not add water-soluble metal salt.
More preferably, in said step a, in fermented liquid, do not add the water-soluble metal salt of following metal: magnesium, calcium, barium, zinc, aluminium or its combination.
In another kind of preference, in said step a, the consumption of lower alcohol is the 10%-25% of fermented liquid.
In another kind of preference, the consumption of lower alcohol is the long-pending 15-25% of gellan gum fermentation liquid.
In another kind of preference, in said step b, the water cut of the flocculation material of said dehydration is 80%-85%.
In another kind of preference, in said step c, the said water consumption of dissolved again is the 60-90% of fermentating liquid volume, preferably 70%-80%.
In another kind of preference, in said steps d, described mineral alkali is selected from down group: sodium hydroxide, Pottasium Hydroxide, yellow soda ash, salt of wormwood or its combination.
In another kind of preference, in said step e, said discoloring agent is an acidic white earth.
In another kind of preference, the consumption of discoloring agent is the 0.5-6wt% of fermented liquid, preferably 1-5wt%.
In another kind of preference, the gel transmittance of described high acyl gellan gum is not less than 70% (like 72-85%).
In another kind of preference, in the described high acyl gellan gum, the content of the water-soluble metal salt of following metal is following: zinc and aluminium do not detect; Total content≤the 20ppm of magnesium, calcium and barium.
In second aspect of the present invention; A kind of transparent high acyl gellan gum is provided; The gel transmittance of said gelling gum is not less than 70% (like 72-85%); And in described high acyl gellan gum, the content of the water-soluble metal salt of following metal is following: zinc and aluminium do not detect (≤10ppm, more preferably≤5ppm; Best≤1ppm); And the total content≤20ppm of magnesium, calcium and barium (preferably≤10ppm).
In another kind of preference, described transparent high acyl gellan gum is to prepare with the method described in the first aspect present invention.
In should be understood that within the scope of the present invention, above-mentioned each technical characterictic of the present invention and specifically described each technical characterictic can mutual combination in (like embodiment) hereinafter, thus constitute new or optimized technical scheme.For example, can make up with the lower limit 1.5 of another preferable range 1.5-2.5 with regard to the upper limit 3.5 of pH 1: 0-3.5, thereby constitute scope 1.5-3.5, vice versa.As space is limited, this tired no longer one by one stating.
Embodiment
The inventor is through extensive and deep research, developed at acidic conditions first and do not use under the situation of salt as flocculation agent, with low cost, prepare the new production process of transparent high acyl gellan gum (being the transparent type high acyl gellan gum) expeditiously.Novel process of the present invention not only can be produced high clarifying high acyl gellan gum, and owing to reduced the usage quantity of alcohol, salt and alkali, has reduced production cost significantly.In addition, novel process has been saved desalinating process, reduces three wastes discharge amount, helps to protect environment.Accomplished the present invention on this basis.
As used herein, term " high clarification high acyl gellan gum ", " transparent high acyl gellan gum " and " transparent type high acyl gellan gum " interchangeable use refer to that all transmittance is greater than 70% high acyl gellan gum.More preferably, in said transparent (type) high acyl gellan gum, the total content of the water-soluble metal salt of metals such as zinc, aluminium, magnesium, calcium, barium is very low.Usually, zinc and aluminium do not detect (≤10ppm, more preferably≤5ppm; Best more preferably≤1ppm); Total content≤the 20ppm of magnesium, calcium and barium (preferably≤10ppm).
At first, the invention provides the method for producing the transparent type high acyl gellan gum, it may further comprise the steps:
(a) flocculation:
The inventive method adopts acid/pure co-coagulation.Regulate the pH to 1.0-3.5 of gellan gum fermentation liquid earlier, add alcohol then, thereby make the flocculation of gelling gum composition, form the liquid stock that contains the gelling gum throw out.
Can be used for the not special restriction of acid of the present invention, can be organic acid or mineral acid, preferred mineral acid, especially hydrochloric acid, sulfuric acid or its combination.
The not special restriction of the concentration of mineral acid is generally 1-5wt%.
A kind of preferred mode be with fermenation raw liquid in whipping process, flow the hydrochloric acid that adds 0.5wt%～3.5wt% concentration to pH be 1.5-3.5; Add about 15-25% volume of ethanol (pressing the volumeter of fermenation raw liquid) then; Thereby make the flocculation of gelling gum composition, form the liquid stock that contains the gelling gum throw out.
Acid of the present invention/pure co-coagulation method can make flocculation more complete, and decon is more, has improved product purity and transparency.
(b) dehydration:
Liquid stock to containing the gelling gum throw out dewaters, the flocculation material (like filter cake) that obtains dewatering.The available ordinary method of wherein dewatering is carried out, and for example carries out with water-removing press.
(c) homogenate:
With the gelling gum filter cake and a certain amount of water mixing homogenate of said dehydration, form homogenate mixture (being the glue of gelling gum).
In this step, the not special restriction of the water yield of adding, the 10-20 of the gelling gum filter cake weight of common said dehydration doubly also can add many slightly water.
Press the volume calculation of fermented liquid, the dissolved water consumption is generally the 60-90% of fermentating liquid volume, preferably 70%-80% again.
Homogenate can be carried out with the conventional method and apparatus in this area.For example, use hollander,, form the homogenate mixture (being also referred to as the pasty liquid material) of pasty state the gelling gum filter cake and the water mixing homogenate of said dehydration.
(d) regulate PH near neutral:
In this step, with alkaline conditioner with homogenate mixture pH regulator to nearly neutral (pH6-7.5, preferably pH6-7).
In this step, the conventional various pH regulator agent in the available this area of pH regulator agent.The representative example of alkaline conditioner comprises (but being not limited to): sodium hydroxide, Pottasium Hydroxide, calcium hydroxide or its combination.Preferred alkaline conditioner is a sodium hydroxide.
(e) decolouring:
In the decolouring step, add carclazyte (like acidic white earth) as discoloring agent, be heated to then (as 90-98 ℃) more than 75 ℃.
Then, to glue mixture filtered while hot, thereby acquisition contains the filtrating of gelling gum.
In this step, various usual manners in available this area and equipment filter.Because when temperature was low, gelling gum can solidify, the temperature of glue mixture should keep comparatively high temps (being generally 70-90 ℃) when therefore filtering, in case gelling gum condenses and hinders filtration.
In addition, before filtering, also can be used on an amount of flocculating aids of interpolation in the glue mixture.The example of flocculating aids commonly used comprises (but being not limited to): zeyssatite, perlite or its combination.
In one type of preference, in the glue mixture, add the 0.5-3.0wt% flocculating aids, filter then.
(f) secondary flocculation and dehydration:
In this step, cool off (for example be cooled to below 50 ℃, preferably be cooled to) a little for the filtrating after the decolouring like room temperature to 50 ℃ after, carry out flocculation treatment once more with regard to available lower alcohol (like ethanol), dewater then, thereby obtain the wet article of gelling gum.
Perhaps, the feed liquid that also contains the gel state gelling gum is carried out press filtration, thereby removes portion of water, obtains gelling gum filter cake (wet article).If select press filtration for use, can use the conventional press filtration device (like pressure filter) in this area to carry out press filtration.After the press filtration, the gelling gum solid content is 15-30% in the filter cake usually.
The measuring method of solid content is measured with ordinary method, for example GB5009.3 weight loss on drying method.
(g) post-processing step such as granulation, drying:
For the gelling gum filter cake after the press filtration, can randomly carry out granulation with usual manner, form granular material.Granulation can be carried out with the conventional method and apparatus in this area, for example uses commercially available tablets press.
Particulate state gelling gum material is carried out drying treatment (for example oven dry), thereby obtain the exsiccant gelling gum.Usually water ratio more preferably is 0.1-15wt% less than 15wt% in the exsiccant gelling gum.Dry can carrying out with the conventional method and apparatus in this area for example used commercially available various drying machines, especially the negative pressure drying machine.
Dried material is pulverized, thereby obtained pulverous gelling gum.Pulverizing can be carried out with the conventional method and apparatus in this area, for example uses commercially available various kibblers.In a preference, material is carried out low-temperature airflow pulverize.
In a preference of the present invention, preparation technology is following:
Fermented liquid is at room temperature used 2.0% hydrochloric acid soln acidifying while stirring, is 2.0 until the pH of material, and consumption is about 10% of fermented liquid, adds 95% ethanol simultaneously, and consumption is 20% of a fermented liquid, and purpose is to make flocculation more complete, improves decolorizing effect simultaneously.About 10 minutes, flocculation was carried out filter-press dehydration after finishing.Material moisture after the dehydration is 80%-85%.The water that adds 70%-80% again stirs dissolving more fast, regulates pH to 6.0-7.0 with 10% sodium hydroxide solution simultaneously; Add 2% acidic white earth, be heated to 90-98 ℃, filter; Obtain white or light yellow clear filtrate; Dewater in 1: 1 ratio with 95% ethanol in cooling back, the article warp drying that wets, pulverize white transparent high acyl gellan gum.
Use
Can make the gelling gum goods of various routines with gelling gum of the present invention, in these gelling gum goods, the content of gelling gum is the 0.01-99wt% of goods gross weight usually, more preferably is 0.1-50wt%.
Representational gelling gum goods comprise (but being not limited to):
(1) food: beverage, cake, jam, jelly, synthesised food, feed for pet, sugar-coat, frosting, milk food prod or bean product etc.;
(2) medicine: collyrium, soft or hard capsule, microcapsule or dressing etc.;
(3) makeup: personal care product or perfume etc.;
(4) Chemicals: film, tackiness agent, toothpaste or air aromatic etc.;
(5) agricultural prods: slow release fertilizer etc.;
(6) other products: mikrobe or plant tissue culture media etc.
The high acyl gellan gum that makes with the inventive method has high purity, transparency advantages of higher, and the technology cost is low.Major advantage of the present invention comprises:
1, acid/pure co-coagulation method makes flocculation more complete, and impurity elimination is more, has improved product purity and transparency.
2, save the usage quantity of salt, reduced pure usage quantity significantly, reduced production cost significantly.
3, save the water of desalinating process and 20%-80%, thereby reduced the three wastes discharge amount of 20%-80%, reduced corresponding energy consumption.
4, use the carclazyte decoloration process instead, compare with gac, decolorizing effect is better, and technology is simple, and polluted product reaches more than 72% the product transmittance, and color and luster is whiter.
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 the restriction scope of the present invention.The experimental technique of unreceipted actual conditions in the following example, usually according to the condition described in the normal condition, or the condition of advising according to manufacturer.Only if indicate in addition, otherwise per-cent and umber are calculated by weight.
Embodiment 1
Obtain to contain the fermenation raw liquid of gelling gum by ordinary method (like the 1 described method of embodiment in the one Chinese patent application 00125858.3).Press following prepared high acyl gellan gum:
Flocculation
To gelling gum first product content is in the fermented liquid of 3900 grams of 16 grams per liters, drips 1.92% hydrochloric acid (about 400ml) while stirring, is 2.0 until the pH of material.Add 95% ethanol 780 grams then, be cooled to room temperature.
Dehydration
Flocculation is carried out filter-press dehydration after finishing, and article 224 grams (material moisture after the dehydration is 80%-85%) must wet.
Glue, decolouring
The wet article of gained add water 3200ml, are neutralized to pH 6.0-7.0 with 10% sodium hydroxide while stirring.Add acidic white earth 60 grams, be heated to 95 ℃, make flocculating aids with zeyssatite, the B suction filtration gets the about 3000ml of light-coloured transparent filtrating.
Dehydration, drying
Treat clear filtrate cooling back (being lower than 50 ℃ gets final product), in 3000ml filtrates, add 95% ethanol 3000ml, wet article are pulverized to such an extent that white transparent high acyl gellan gum 40.7 restrains through oven dry.
Performance test
To the gelling gum of preparation among the embodiment 1, measure its performance with ordinary method.
The result is as shown in table 1 below:
Table 1 sample detected result and measuring method:
| Outward appearance | This white | Measuring method |
| Weight loss on drying | ＜15％ | GB5009.3 |
| Transmittance | ＞75％ | Relatively (detect) with pure water with the ultraviolet spectrometry protractor |
| Zinc | ＜1ppm | |
| Aluminium | ＜1ppm | |
| Magnesium, calcium and barium total amount | ＜20ppm |
Embodiment 2:
Repeat embodiment 1, difference only is: the sulfuric acid with 2.0% replaces hydrochloric acid to make flocculation agent.
As a result, get high acyl gellan gum finished product 38.1 grams.
Through measuring transmittance＞72%.Zinc and aluminium do not detect (＜5ppm); Total content＜the 10ppm of magnesium, calcium and barium.
Embodiment 3:
Repeat embodiment 1, difference only is: replace 95% ethanol to make flocculation agent with 98% Virahol.
As a result, get high acyl gellan gum finished product 42.4 grams.
Through measuring transmittance＞80%.Zinc and aluminium do not detect (＜5ppm); Total content＜the 20ppm of magnesium, calcium and barium.
Embodiment 4:
Repeat embodiment 1, difference only is: do not add zeyssatite (flocculating aids).
As a result, get high acyl gellan gum finished product 41.0 grams.
Through measuring transmittance＞72%.Zinc and aluminium do not detect (＜5ppm); Total content＜the 20ppm of magnesium, calcium and barium.
Embodiment 5:
Repeat embodiment 1, difference only is: add acidic white earth 40 grams.
As a result, get high acyl gellan gum finished product 41.2 grams.
Through measuring transmittance＞74%.Zinc and aluminium do not detect (＜5ppm); Total content＜the 20ppm of magnesium, calcium and barium.
All documents in that the present invention mentions are all quoted as a reference in this application, are just quoted such as a reference separately as each piece document.Should be understood that in addition after having read above-mentioned teachings of the present invention, those skilled in the art can do various changes or modification to the present invention, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Claims (8)
1. a method for preparing the transparent type high acyl gellan gum is characterized in that, described method comprises step:
A. gellan gum fermentation liquid is mixed with mineral acid and lower alcohol and carry out flocculation treatment, thereby obtain to contain the flocculation material of gelling gum throw out;
B. described flocculation material is dewatered, obtain the flocculation material of dehydration;
C. the flocculation material adding water to dehydration dissolves again, thereby obtains to contain the glue of gelling gum;
D. regulate the pH to 6-7 of the glue of said gelling gum with mineral alkali;
E. the adding discoloring agent decolours and filters in said glue, obtains to contain the filtrating of gelling gum;
F. the said filtrating that contains gelling gum is carried out flocculation treatment, and dehydration once more, the wet article of gelling gum that dewater obtained; With
G. the wet article of described gelling gum are carried out drying, obtain transparent type high acyl gellan gum product;
In said step a, in fermented liquid, do not add water-soluble metal salt;
Wherein, described lower alcohol is selected from down group: ethanol, Virahol or its combination.
2. the method for claim 1 is characterized in that, in said step a, mineral acid is selected from down group: hydrochloric acid, sulfuric acid or its combination.
3. the method for claim 1 is characterized in that, in said step a, regulates the pH to 1.0-3.5 of fermented liquid with mineral acid.
4. the method for claim 1 is characterized in that, in said step a, the consumption of lower alcohol is the 10%-25% of fermented liquid.
5. the method for claim 1 is characterized in that, in said step c, the said water consumption of dissolved again is the 60-90% of fermentating liquid volume,
6. the method for claim 1 is characterized in that, in said step c, the said water consumption of dissolved again is the 70%-80% of fermentating liquid volume.
7. the method for claim 1 is characterized in that, in said steps d, described mineral alkali is selected from down group: sodium hydroxide, Pottasium Hydroxide, yellow soda ash, salt of wormwood or its combination.
8. the method for claim 1 is characterized in that, in said step e, said discoloring agent is an acidic white earth.
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| EP2925791B1 (en) | 2012-12-03 | 2017-03-22 | Colgate-Palmolive Company | Manufacturing processes for gellan gum-based fluid gels |
| CN103509844B (en) * | 2013-08-09 | 2015-05-13 | 新疆阜丰生物科技有限公司 | Low-acyl gellan gum extracting method |
| CN103436587B (en) * | 2013-08-23 | 2015-05-20 | 新疆阜丰生物科技有限公司 | Purifying method of transparent type high-acyl gellan gum |
| CN103409492B (en) * | 2013-08-23 | 2015-05-13 | 新疆阜丰生物科技有限公司 | Method for extracting transparent low-acyl gellan gum |
| CN108690143A (en) | 2017-04-07 | 2018-10-23 | 帝斯曼知识产权资产管理有限公司 | A kind of production method of high transparency low-acyl gellan gum |
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| CN101191138A (en) * | 2006-11-28 | 2008-06-04 | 尹洪波 | Method for producing gellan gum finished product from gellan gum fermentation liquor |
| AU2008309218A1 (en) * | 2007-10-10 | 2009-04-16 | Nairsons Flavourhouse Cc | Method of producing acid stable protein products and products so produced |
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| CN1635133A (en) * | 2004-11-19 | 2005-07-06 | 张禹 | Gellan gum post-extraction method |
| CN1687437A (en) * | 2005-03-25 | 2005-10-26 | 张禹 | Method of high post extraction of acyl Gellan |
| CN101062957A (en) * | 2006-04-24 | 2007-10-31 | 上海众伟生化有限公司 | Gellan gum without organic solvent and production technique thereof |
| CN101191138A (en) * | 2006-11-28 | 2008-06-04 | 尹洪波 | Method for producing gellan gum finished product from gellan gum fermentation liquor |
| AU2008309218A1 (en) * | 2007-10-10 | 2009-04-16 | Nairsons Flavourhouse Cc | Method of producing acid stable protein products and products so produced |
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