CN103205471B - Xanthan gum preparation method suitable for high-concentration multivalent ion liquid - Google Patents
Xanthan gum preparation method suitable for high-concentration multivalent ion liquid Download PDFInfo
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- CN103205471B CN103205471B CN201310159309.0A CN201310159309A CN103205471B CN 103205471 B CN103205471 B CN 103205471B CN 201310159309 A CN201310159309 A CN 201310159309A CN 103205471 B CN103205471 B CN 103205471B
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Abstract
The invention relates to a xanthan gum preparation method suitable for a high-concentration multivalent ion liquid, and belongs to the technical field of the production of xanthan gum. The process comprises a fermenting stage and an extracting stage. The process comprises the following steps of: reducing PH and temperature in the fermenting process, acidifying in the fermenting liquid extracting process; then, repeatedly crystallizing twice by alcohols for cooling; and performing solid-liquid separation, drying and crushing to obtain the xanthan gum product. The product can completely release viscosity in 5% of divalent ion liquid and 3% of trivalent ion liquid. Compared with common xanthan gum product lower than that of 2% of divalent ion liquid and 1% of trivalent ion liquid, the market use is greatly expanded.
Description
Technical field
The invention belongs to xanthan gum production technical field, be specifically related to a kind of xanthan gum preparation technology who is applicable to high density polyvalent ion solution.
Background technology
Xanthan gum claims again yellow glue, xanthan gum, is a kind of biological poly-and thing, is a kind of pale yellow powder.Xanthan gum can be dissolved in cold water and hot water, there is high viscosity, high acid-and base-resisting, salt characteristic, high heat-resistant stability, suspension, thixotropy etc., be often used as thickening material, emulsifying agent, suspension agent, stablizer, there are wide market outlook, be widely used in the fields such as daily-use chemical industry, food, medicine, oil recovery, weaving, pottery, printing and dyeing.But the xanthan gum product of current domestic scale operation can only be applicable to the salt ion solution of lower concentration, but along with rising or the low price ion of salt ionic concentration are transformed into high valence ion, the rheological of its xanthan gum and viscoelastic performance reduce, result of use is undesirable, thereby has limited the scope of application of xanthan gum.The xanthan gum product that can adapt at present high density a polyvalent salt solion is also step-sizing a small amount of xanthan gum out in process of production, cause like this specific aim of production to reduce, expended the time, man power and material, also improved the production cost of extraordinary xanthan gum product.
The performance of xanthan gum depends primarily on the preparation technology of xanthan gum and the selection of bacterial strain, and the research carrying out for the preparation technology of xanthan gum who is applicable to high density polyvalent ion solution in prior art is very rarely seen.In order to overcome the deficiencies in the prior art, the xanthan gum product that urgently needs to solve existing scale operation is suitable for the problem of weak effect in high density polyvalent ion solution.
Summary of the invention
The xanthan gum product that the object of the invention is to solve existing scale operation yields poorly and in high density polyvalent ion solution, is suitable for the problem of weak effect, make not only output raising of xanthan gum product, and in the solution of high density polyvalent ion, there is good rheological, visco-elasticity and Mud Property characteristic.
The present invention is achieved through the following technical solutions:
An xanthan gum preparation technology who is applicable to high density polyvalent ion solution, comprises the steps:
An xanthan gum preparation technology who is applicable to high density polyvalent ion solution, it comprises the steps:
1), obtaining liq fermention medium (massfraction): sucrose 2.0%, citric acid 0.42%, W-Gum 0.6%, KCl0.1%, NaH
2pO
40.05%, MgSO
40.2%, Ca (H
2pO
4)
20.1%, surplus is water;
2), after aforesaid liquid fermention medium preparation, the pH value of adjusting substratum with the KOH solution of 2mol/L is to 7.4-7.5, sterilizing 40 minutes at 120 ℃ is inoculated bacterium liquid after being cooled to 34 ℃, inoculum size is 5.0%, ferments;
3), fermentation stage: ferment after 10 hours, regulate the pH value of fermented liquid at 6.97.1, temperature is controlled at 32-34 ℃, ferments after 40 hours, regulates fermentating liquid PH value at 5.5-5.7, and temperature is controlled at 32 ℃; Incubation time 65 hours, obtains fermented liquid;
4), the extraction stage:
A) in step 3) to add massfraction in the xanthan gum fermentation broth that obtains be 5.0% acid, and stir, control pH value at 4.8-5;
B) in solution, add ethanol or Virahol, in control solution, the concentration of volume percent of ethanol or Virahol, at 55%-60%, stirs 45 minutes;
C) feed liquid step b) being generated is carried out solid-liquid separation;
D) step c) is separated to the solid obtaining and join in ethanol or Virahol again, in control solution, the concentration of volume percent of ethanol or Virahol, at 60%-65%, stirs 40 minutes;
E) by steps d) finish mix liquid carries out solid-liquid separation again, and gained solid is dried at 65 ℃;
F) dried solid is pulverized, obtained being applicable to the xanthan gum of high density polyvalent ion solution.
Preferably, described bacterium liquid is Xanthomonas campestris liquid.
Preferably, described bacterium liquid is composite bacteria liquid, and described composite bacteria liquid is mixed according to volume ratio by Xanthomonas campestris liquid and Issatchenkia orientalis bacterium liquid at 2: 1.
Preferably, described step 4) in acid be the wherein a kind of of phosphoric acid, hydrochloric acid, nitric acid, sulfuric acid or acetic acid.
The beneficial effect that the present invention obtains:
1, the xanthan gum product that the present invention obtains can be used in 5% divalent ion solution and 3% trivalent ion solution, in solution, keeping good rheology solvability and shear viscosity characteristic, compare the coventional type xanthan gum product that can only adapt to lower than 2% divalent ion and 1% trivalent ion solution, expanded the scope of application of xanthan gum product; It can be applied in avoids causing flocculation in the solution that contains polyvalent ion and produces precipitation.In petroleum drilling, xanthan gum product prepared by the inventive method more can be applicable in calcium treated drilling fluid, in the time of the calcium treated drilling fluid of 10.0g/L, there is outstanding rheological and superior Mud Property characteristic than the xanthan gum of other kinds, can greatly improve drilling speed, make drilling fluid there is higher pit shaft and clean effect and suspending power, its temperature resistance ability meets 121 ℃, and in use the impact of performance of xanthan gum can variation, can reduce the usage quantity of xanthan gum, save drilling cost.The purposes that also can contain multivalence macroion solution as cement slurrying etc. for other.
2, the application carries out creative experiments to xanthan gum generation bacterium a large amount of in prior art, finds through many experiments, and two kinds of suitable bacterium act synergistically jointly, can improve the output of xanthan gum.
3, in preparation technology of the present invention, adopted specific Technology, for example gradient PH and temperature, the repeatedly technology such as solid-liquid separation, has improved the performance of xanthan gum, has greatly improved the high concentration ion adaptedness of xanthan gum.
Embodiment
Below employing specific embodiment is further explained the present invention, but should regard the restriction to initiative spirit of the present invention as.
Embodiment 1
An xanthan gum preparation technology who is applicable to high density polyvalent ion solution, it comprises the steps:
1), obtaining liq fermention medium (by weight): sucrose 2.0%, citric acid 0.42%, W-Gum 0.6%, KCl0.1%, NaH
2pO
40.05%, MgSO
40.2%, Ca (H
2pO
4)
20.1%, surplus is water;
2), after aforesaid liquid fermention medium preparation, adjust the pH value to 7.5 of substratum with the KOH solution of 2mol/L, sterilizing 40 minutes at 120 ℃, (concentration is 1 × 10 to inoculate Xanthomonas campestris liquid after being cooled to 34 ℃
8individual/mL), inoculum size is 5.0%, ferments;
3), fermentation stage: ferment after 10 hours, regulate the pH value of fermented liquid 7.1, temperature is controlled at 34 ℃, ferments after 40 hours, regulates fermentating liquid PH value 5.7, and temperature is controlled at 32 ℃; Incubation time 65 hours, obtains fermented liquid;
4), the extraction stage:
A) in step 3) to add massfraction in the xanthan gum fermentation broth that obtains be 5.0% phosphoric acid, and stir, control pH value 4.8;
B) in solution, add ethanol, control the concentration of volume percent of ethanol in solution 55%, stir 45 minutes;
C) feed liquid step b) being generated is carried out solid-liquid separation;
D) step c) is separated to the solid obtaining and join again in ethanol, control the concentration of volume percent of ethanol in solution 60%, stir 40 minutes;
E) by steps d) finish mix liquid carries out solid-liquid separation again, and gained solid is dried at 65 ℃;
F) dried solid is pulverized, obtained being applicable to the xanthan gum of high density polyvalent ion solution.
Embodiment 2
An xanthan gum preparation technology who is applicable to high density polyvalent ion solution, it comprises the steps:
1), obtaining liq fermention medium (by weight): sucrose 2.0%, citric acid 0.42%, W-Gum 0.6%, KCl0.1%, NaH
2pO
40.05%, MgSO
40.2%, Ca (H
2pO
4)
20.1%, surplus is water;
2), after aforesaid liquid fermention medium preparation, adjust the pH value to 7.4 of substratum with the KOH solution of 2mol/L, sterilizing 40 minutes at 120 ℃, inoculates composite bacteria liquid after being cooled to 34 ℃, inoculum size is 5.0%, ferments;
This composite bacteria liquid is mixed by the volume ratio of 2: 1 by Xanthomonas campestris liquid Xanthomonas.SP CGMCCNO:3624 (CN101906390A) and Issatchenkia orientalis bacterium liquid (Issatchenkia orientalis Z1) CCTCC M2010167 (referring to CN102102084), wherein, in Xanthomonas campestris liquid and Issatchenkia orientalis bacterium liquid, the concentration of thalline is all about 1 × 10
8individual/mL;
3), fermentation stage: ferment after 10 hours, regulate the pH value of fermented liquid 6.9, temperature is controlled at 32 ℃, ferments after 40 hours, regulates fermentating liquid PH value 5.5, and temperature is controlled at 30 ℃; Incubation time 65 hours, obtains fermented liquid;
4), the extraction stage:
A) in step 3) to add massfraction in the xanthan gum fermentation broth that obtains be 5.0% phosphoric acid, and stir, control pH value 5;
B) in solution, add Virahol, control the concentration of volume percent of Virahol in solution 60%, stir 45 minutes;
C) feed liquid step b) being generated is carried out solid-liquid separation;
D) step c) is separated to the solid obtaining and join again in Virahol, control the concentration of volume percent of Virahol in solution 65%, stir 40 minutes;
E) by steps d) finish mix liquid carries out solid-liquid separation again, and gained solid is dried at 65 ℃;
F) dried solid is pulverized, obtained being applicable to the xanthan gum of high density polyvalent ion solution.
Embodiment 3
The performance perameter of implementing the xanthan gum of 1 and 2 preparations detects: xanthan gum prepared by more solito.Utilize respectively 5% ferric chloride Solution or 3% iron(ic) chloride to configure 1% xanthan gum solution, measure solution at 100s for 25 ℃
-1viscosity under shearing rate; And detect gum yield.Referring to table 1
Table 1
Conclusion: the xanthan gum product that the present invention obtains can be used in 5% divalent ion solution and 3% trivalent ion solution, in solution, keeping good rheology solvability and shear viscosity characteristic, compare the coventional type xanthan gum product that can only adapt to lower than 2% divalent ion and 1% trivalent ion solution, expanded the scope of application of xanthan gum product.
Finally, it is also to be noted that, what more than enumerate is only several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, can also have many distortion.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention, all should think protection scope of the present invention.
Claims (1)
1. an xanthan gum preparation technology who is applicable to high density polyvalent ion solution, it comprises the steps:
1), obtaining liq fermention medium: sucrose 2.0%, citric acid 0.42%, W-Gum 0.6%, KCl0.1%, NaH
2pO
40.05%, MgSO
40.2%, Ca (H
2pO
4)
20.1%, surplus is water;
2), after aforesaid liquid fermention medium preparation, by the pH value of the KOH solution adjustment substratum of 2mol/L, to 7.4-7.5, sterilizing 40 minutes at 120 ℃, inoculates bacterium liquid after being cooled to 34 ℃, inoculum size is 5.0%, ferments;
3), fermentation stage: ferment after 10 hours, regulate the pH value of fermented liquid at 6.9-7.1, temperature is controlled at 32-34 ℃, ferments after 40 hours, regulates fermented liquid pH value at 5.5-5.7, and temperature is controlled at 32 ℃; Incubation time 65 hours, obtains fermented liquid; 4), the extraction stage:
A) in step 3) to add massfraction in the xanthan gum fermentation broth that obtains be 5.0% acid, and stir, control pH value at 4.8-5;
B) in solution, add ethanol or Virahol, in control solution, the concentration of volume percent of ethanol or Virahol, at 55%-60%, stirs 45 minutes;
C) feed liquid step b) being generated is carried out solid-liquid separation;
D) step c) is separated to the solid obtaining and join in ethanol or Virahol again, in control solution, the concentration of volume percent of ethanol or Virahol, at 60%-65%, stirs 40 minutes;
E) by steps d) finish mix liquid carries out solid-liquid separation again, and gained solid is dried at 65 ℃;
F) dried solid is pulverized, obtained being applicable to the xanthan gum of high density polyvalent ion solution;
Described bacterium liquid is composite bacteria liquid, and described composite bacteria liquid is mixed according to volume ratio by Xanthomonas campestris liquid and Issatchenkia orientalis bacterium liquid at 2: 1.
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| CN105463050B (en) * | 2015-12-18 | 2019-02-12 | 内蒙古阜丰生物科技有限公司 | A kind of natural additive for foodstuff xanthan gum and its preparation process |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101186654A (en) * | 2007-12-12 | 2008-05-28 | 山东阜丰生物科技开发有限公司 | Method for extracting xanthan gum used for calcium treated drilling fluid |
| CN101185486A (en) * | 2007-12-12 | 2008-05-28 | 山东阜丰生物科技开发有限公司 | Method for producing xanthan gum used for preparing beverage |
| CN101560537A (en) * | 2009-05-19 | 2009-10-21 | 四川恒益科技有限公司 | Fermentation method for producing high viscocity xanthan gum by xanthomonas campestris |
| WO2012030651A1 (en) * | 2010-08-31 | 2012-03-08 | Cp Kelco U.S., Inc. | Xanthan gum with fast hydration and high viscosity |
-
2013
- 2013-04-26 CN CN201310159309.0A patent/CN103205471B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101186654A (en) * | 2007-12-12 | 2008-05-28 | 山东阜丰生物科技开发有限公司 | Method for extracting xanthan gum used for calcium treated drilling fluid |
| CN101185486A (en) * | 2007-12-12 | 2008-05-28 | 山东阜丰生物科技开发有限公司 | Method for producing xanthan gum used for preparing beverage |
| CN101560537A (en) * | 2009-05-19 | 2009-10-21 | 四川恒益科技有限公司 | Fermentation method for producing high viscocity xanthan gum by xanthomonas campestris |
| WO2012030651A1 (en) * | 2010-08-31 | 2012-03-08 | Cp Kelco U.S., Inc. | Xanthan gum with fast hydration and high viscosity |
Non-Patent Citations (4)
| Title |
|---|
| 分段控温黄原胶发酵过程;朱圣东等;《石油化工高等学校学报》;20051231;第18卷(第4期);24-26 * |
| 朱圣东等.分段控温黄原胶发酵过程.《石油化工高等学校学报》.2005,第18卷(第4期),24-26. |
| 杨澴等.黄原胶发酵及提取工艺的优化研究.《食品工业》.2008,(第6期),20-23. |
| 黄原胶发酵及提取工艺的优化研究;杨澴等;《食品工业》;20081220(第6期);20-23 * |
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