CN102659954A - Separation and purification technology of xanthan gum - Google Patents
Separation and purification technology of xanthan gum Download PDFInfo
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- CN102659954A CN102659954A CN2011104227627A CN201110422762A CN102659954A CN 102659954 A CN102659954 A CN 102659954A CN 2011104227627 A CN2011104227627 A CN 2011104227627A CN 201110422762 A CN201110422762 A CN 201110422762A CN 102659954 A CN102659954 A CN 102659954A
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Abstract
The invention discloses a separation and purification technology of xanthan gum. The method comprises the following steps: diluting a xanthan gum zymotic fluid, and carrying out perlite filtering, neutral protease degradation, enzyme deactivation, condensation by ultrafiltration, precipitation with ethanol, and centrifugation drying to obtain a xanthan gum product of high quality. The separation and purification technology of xanthan gum of the invention is characterized by a simple extraction process, convenient operation, low production cost, and product with light transmittance higher than 85% and purity higher than 95%, and is suitable for industrial scale production.
Description
Technical field
The invention belongs to the XG 550 production technical field, be specifically related to a kind of from fermented liquid the method for separation and purification XG 550.
Background technology
XG 550 (Xanthan gum) is an industrial scale maximum and purposes microbial polysaccharide the most widely in the world at present; It is a kind of exocellular polysaccharide that utilizes glucide to produce by Xanthomonas campestris (Xanthomonas campestris); Ability with good water-solubility, tackifying, pseudo-plasticity and acid and alkali-resistance, salt tolerant and anti-enzymolysis; Often be used as thickening material, emulsifying agent, suspension agent, stablizer, be widely used in fields such as chemical industry, food, pottery, medicine, weaving, oil recovery, printing and dyeing, coating, explosive, metallurgy, papermaking, fire extinguishing, agricultural chemicals and makeup.
Along with the expansion of XG 550 range of application, throughput global and domestic XG 550 rises year by year, and market demand every year of XG 550 is with 8% speed increment, so the throughput of XG 550 also need continue to strengthen, and market also belongs to the high speed growth stage.But the leavened prod quality of XG 550 is low at present, and product glue rate is low, has caused production cost higher, the more expensive development and application that waits the restriction XG 550 of the price of XG 550.The production technique of China's XG 550 is backward relatively, and production throughput such as the fine chemistry industry level XG 550 of high added value, transparent type XG 550, various tailored version XG 550 are relatively weaker; Indexs such as fermentation capacity, polysaccharide transformation efficiency have been compared big gap with international most advanced level.
XG 550 production comprises fermentation and downstream processing two portions, and comparatively speaking, the downstream processing that XG 550 is produced (separation, purifying and process finished product) is studied less, and downstream process required expense and account for 50%～60% of production cost.High-quality yellow virgin rubber such as clear XG 550, instant type XG 550 (these product import prices are more than the twice of domestic food level XG 550 price) etc., its downstream processing charges is higher.Therefore, the downstream course of processing directly determines the quality and the production cost of XG 550, and the downstream processing technology has become the critical process that XG 550 is produced.
Except the XG 550 that contains low concentration (2%～5%), also have a large amount of mycelium, residual sugar, inorganic salt and other impurity in the xanthan gum fermentation broth, different separation purification method will determine performance, quality and the purposes of XG 550.At present, the process method of the separation and purification of xanthan gum product mainly contains direct drying method, organic solvent precipitation method, salt precipitation method and ultra-filtration membrane partition method etc., but on using, all receives the restriction of condition separately.Remove thalline remains in the xanthan gum solution how to greatest extent, at an easy rate and from the solid impurity of fermentation substrate, XG 550 is concentrated to a certain degree to reduce dry used energy, precipitation agent consumption and regeneration expense, be the problem that exists in the present XG 550 aftertreatment.
Summary of the invention
The object of the present invention is to provide a kind of method of producing the high-quality transparent xanthan gum, to overcome the deficiency of prior art.
To achieve these goals, the present invention adopts the technology of separation and purification XG 550 from fermented liquid, may further comprise the steps:
(1) dilution: water is with 1～2 times of xanthan gum fermentation broth dilution;
(2) perlite filters: adopt the pearlite filtering aid filtering fermentating liquid, usage quantity is 10～30g/L, can effectively a large amount of somatic cells that exists in the fermented liquid and other insolubless be removed with perlite;
(3) neutral protease is handled: perlitic filtered solution is transferred pH to 7.0; Every liter of filtrating is added the neutral protease of 10000～100000U; 45～50 ℃ of insulation 1～2h; Neutral protease is handled protein insolubless such as can removing the thalline remains, makes the XG 550 of gained have viscosity and transparence preferably, improves product gas purity;
(4) enzyme that goes out is handled: the fermented liquid that enzyme is handled adjusts the temperature to 80～100 ℃, and insulation 20～60min enzyme that goes out is lived;
(5) ultrafiltration and concentration: adopting the aperture is the filter membrane of 0.2～0.4 μ m, and the fermented liquid that enzyme is handled carries out ultrafiltration and concentration, and filtrate can be reused for the fermented liquid pre-treatment after reverse-osmosis treated---dilution;
(6) ethanol sedimentation: ultrafiltration and concentration liquid is added in 95% ethanol of 2～3 times of volumes, constantly stir, not sticking to solution, centrifugal collecting precipitation reclaims ethanol;
(7) finished product: 75～85 ℃ of dryings, pulverizing promptly get purity greater than 95% xanthan gum product.
Effect of the present invention is:
A, when xanthan gum fermentation broth is carried out pre-treatment; Integrated use perlite filtration method and enzyme liberating method, perlite is more inexpensive more efficient than zeyssatite, earlier with both economical perlite filtering fermentating liquid; Just can remove residual dead bacterium with the enzyme of less amount; More more economical than directly handling fermented liquid with enzyme usually, both combine, and more to reduce impurity residual, effectively improved the quality of XG 550;
It all is in fermented liquid, directly to add ethanol sedimentation that B, tradition are produced XG 550; Consume a large amount of reagent; And the present invention adopts ultrafiltration and concentration to the fermented liquid through pre-treatment; XG 550 content has a more substantial increase in the liquid concentrator, can save amount of ethanol in the separation and purification process widely, effectively reduces cost;
C, the filtrate of ultrafiltration carried out reverse-osmosis treated after, can be reused for the first step of separation and purification---in the dilution fermented liquid, effectively reduced the generation of wastewater flow rate.
The method of separation and purification XG 550 of the present invention, preparation technology is simple, easy to operate, extraction cost is low, yield is high, transmittance is high, the xanthan gum product that the present invention is prepared, content is that xanthan gum solution transmittance when wavelength is 600nm of 1% is higher than 85%.
Description of drawings
Accompanying drawing 1 is with the xanthan gum fermentation broth dilution, carries out perlite filtration, neutral protein enzyme liberating, go out enzyme work, ultrafiltration and concentration, ethanol sedimentation, whiz, obtains the process flow sheet of high-quality xanthan gum product.
Embodiment
Propose following instance and be used to explain the present invention, but content of the present invention is not limited thereto.
Embodiment 1
After 1 times of 1L fermented liquid dilution, to filter with the 10g/L pearlite filtering aid, the filtrating that obtains is transferred pH to 7.0; Add neutral protease 200000U; 45 ℃ of insulation 1h are to decompose the thalline do not eliminate, and the fermented liquid that enzyme is handled adjusts the temperature to 80 ℃, and the insulation 20min enzyme that goes out is lived.Adopting the aperture is the filter membrane of 0.2 μ m; Perlitic filtered solution is carried out ultrafiltration and concentration to 0.5L; Ultrafiltration and concentration liquid is added in 1L 95% ethanol; It is not sticking constantly to stir deposition XG 550 to solution, and centrifugal collecting precipitation, drying, grinding promptly get purity 95.26%, transmittance 85.31% xanthan gum product.
Embodiment 2
After 1 times of 5L fermented liquid dilution, to filter with the 20g/L pearlite filtering aid, the filtrating that obtains is transferred pH to 7.0; Add neutral protease 400000U; 45 ℃ of insulation 1.5h are to decompose the thalline do not eliminate, and the fermented liquid that enzyme is handled adjusts the temperature to 90 ℃, and the insulation 40min enzyme that goes out is lived.Adopting the aperture is the filter membrane of 0.3 μ m, and perlitic filtered solution is carried out ultrafiltration and concentration to 2.5L, and filtrate can be reused for the fermented liquid pre-treatment after reverse-osmosis treated---dilution.Ultrafiltration and concentration liquid is added in 5L 95% ethanol, and it is not sticking constantly to stir deposition XG 550 to solution, reclaims ethanol.Collecting precipitation, drying, pulverizing promptly get purity and are 95.58%, transmittance is 85.97% xanthan gum product.
Embodiment 3
After 1 times of 10L fermented liquid dilution, to filter with the 30g/L pearlite filtering aid, the filtrating that obtains is transferred pH to 7.0; Add neutral protease 200,000 U; 50 ℃ of insulation 2h are to decompose the thalline do not eliminate, and the fermented liquid that enzyme is handled adjusts the temperature to 100 ℃, and the insulation 60min enzyme that goes out is lived.Adopting the aperture is the filter membrane of 0.4 μ m, and perlitic filtered solution is carried out ultrafiltration and concentration to 4L, and filtrate can be reused for the fermented liquid pre-treatment after reverse-osmosis treated---dilution.Ultrafiltration and concentration liquid is added in 8L 95% ethanol, constantly stir the deposition XG 550 to dissolving
Embodiment
Propose following instance and be used to explain the present invention, but content of the present invention is not limited thereto.
Embodiment 1
After 1 times of 1L fermented liquid dilution, to filter with the 10g/L pearlite filtering aid, the filtrating that obtains is transferred pH to 7.0; Add neutral protease 200000U; 45 ℃ of insulation 1h are to decompose the thalline do not eliminate, and the fermented liquid that enzyme is handled adjusts the temperature to 80 ℃, and the insulation 20min enzyme that goes out is lived.Adopting the aperture is the filter membrane of 0.2 μ m; Perlitic filtered solution is carried out ultrafiltration and concentration to 0.5L; Ultrafiltration and concentration liquid is added in 1L 95% ethanol; It is not sticking constantly to stir deposition XG 550 to solution, and centrifugal collecting precipitation, drying, grinding promptly get purity 95.26%, transmittance 85.31% xanthan gum product.
Embodiment 2
After 1 times of 5L fermented liquid dilution, to filter with the 20g/L pearlite filtering aid, the filtrating that obtains is transferred pH to 7.0; Add neutral protease 400000U; 45 ℃ of insulation 1.5h are to decompose the thalline do not eliminate, and the fermented liquid that enzyme is handled adjusts the temperature to 90 ℃, and the insulation 40min enzyme that goes out is lived.Adopting the aperture is the filter membrane of 0.3 μ m, and perlitic filtered solution is carried out ultrafiltration and concentration to 2.5L, and filtrate can be reused for the fermented liquid pre-treatment after reverse-osmosis treated---dilution.Ultrafiltration and concentration liquid is added in 5L 95% ethanol, and it is not sticking constantly to stir deposition XG 550 to solution, reclaims ethanol.Collecting precipitation, drying, pulverizing promptly get purity and are 95.58%, transmittance is 85.97% xanthan gum product.
Embodiment 3
After 1 times of 10L fermented liquid dilution, to filter with the 30g/L pearlite filtering aid, the filtrating that obtains is transferred pH to 7.0; Add neutral protease 200,000 U; 50 ℃ of insulation 2h are to decompose the thalline do not eliminate, and the fermented liquid that enzyme is handled adjusts the temperature to 100 ℃, and the insulation 60min enzyme that goes out is lived.Adopting the aperture is the filter membrane of 0.4 μ m, and perlitic filtered solution is carried out ultrafiltration and concentration to 4L, and filtrate can be reused for the fermented liquid pre-treatment after reverse-osmosis treated---dilution.Ultrafiltration and concentration liquid is added in 8L 95% ethanol, constantly stir the deposition XG 550 to dissolving.
Claims (9)
1. the method for a separation and purification XG 550 from fermented liquid is characterized in that:
(1) fermented liquid dilution: the dilute with water xanthan gum fermentation broth, to reduce viscosity;
(2) perlite filters: with the pearlite filtering aid filtering fermentating liquid, usage quantity is 10～30g/L;
(3) neutral protease is handled: filtered liq is transferred pH to 7.0, and every liter of filtrating is added the neutral protease of 10000～100000U, and 45～50 ℃ of insulation 1～2h are to decompose the thalline that does not eliminate;
(4) enzyme that goes out is lived: the fermented liquid that enzyme is handled adjusts the temperature to 80～100 ℃, and insulation 20～60min enzyme that goes out is lived;
(5) ultrafiltration and concentration: adopting the aperture is the filter membrane of 0.2～0.4 μ m, and the fermented liquid that enzyme is handled carries out ultrafiltration and concentration;
(6) ethanol sedimentation: ultrafiltration and concentration liquid is added in 95% ethanol of 2～3 times of volumes, constantly stir, not sticking to solution, centrifugal collecting precipitation reclaims ethanol;
(7) finished product: 75～85 ℃ drying precipitated, obtains fine XG 550 finished product after the pulverizing.
2. method according to claim 1 is characterized in that described fermented liquid extension rate is 1～2 times.
3. method according to claim 1 is characterized in that describedly with the pearlite filtering aid filtering fermentating liquid, and the perlite usage quantity is 10～30g/L, is advisable with 15～25g/L;
4. method according to claim 1 is characterized in that the neutral protease that described every liter of filtrating is added is 10000～100000U, is advisable with 50000～80000U, and soaking time is advisable with 1.5～2h.
5. method according to claim 1 is characterized in that the described enzyme that goes out temperature alive is 80～100 ℃, insulation 20～60min.
6. method according to claim 1 is characterized in that it is the filter membrane of 0.2～0.4 μ m that described ultrafiltration and concentration adopts the aperture.
7. method according to claim 1, the volume ratio that it is characterized in that described ethanol and liquid concentrator is 2: 1～3: 1.
8. method according to claim 1 is characterized in that described drying temperature is 75～85 ℃.
9. method according to claim 1 is characterized in that gained xanthan gum product transmittance is higher than 85%, and purity is greater than 95%.
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| CN2011104227627A CN102659954A (en) | 2011-12-16 | 2011-12-16 | Separation and purification technology of xanthan gum |
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| CN2011104227627A CN102659954A (en) | 2011-12-16 | 2011-12-16 | Separation and purification technology of xanthan gum |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105646731A (en) * | 2016-04-05 | 2016-06-08 | 浙江立恩生物科技有限公司 | Method for preparing high-quality biological polysaccharide |
| CN109796540A (en) * | 2019-02-26 | 2019-05-24 | 湖北葛店人福药用辅料有限责任公司 | A kind of refining methd of pharmaceutical grade xanthan gum |
-
2011
- 2011-12-16 CN CN2011104227627A patent/CN102659954A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105646731A (en) * | 2016-04-05 | 2016-06-08 | 浙江立恩生物科技有限公司 | Method for preparing high-quality biological polysaccharide |
| CN105646731B (en) * | 2016-04-05 | 2017-12-19 | 浙江立恩生物科技有限公司 | A kind of method for preparing high-quality biological polysaccharide |
| CN109796540A (en) * | 2019-02-26 | 2019-05-24 | 湖北葛店人福药用辅料有限责任公司 | A kind of refining methd of pharmaceutical grade xanthan gum |
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Application publication date: 20120912 |