CN1283649C - Preparation method of refining xylan - Google Patents
Preparation method of refining xylan Download PDFInfo
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- CN1283649C CN1283649C CN 200510039239 CN200510039239A CN1283649C CN 1283649 C CN1283649 C CN 1283649C CN 200510039239 CN200510039239 CN 200510039239 CN 200510039239 A CN200510039239 A CN 200510039239A CN 1283649 C CN1283649 C CN 1283649C
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Abstract
The present invention relates to the field of xylan preparation, particularly to a preparation method of refined xylan. The method concretely comprises: A, alkaline solution is used for pumping alkaline soluble substances in raw material; B, alcohol is added in alkaline pumping solution; after the alcohol is uniformly mixed, acid is used for adjusting the pH of the solution; sediments as coarse xylan are collected by centrifugation or filtration; C, the alcohol is used for washing the coarse xylan at least once; obtained sediments are refined xylan. The technologic process of the present invention of preparing the xylan has the advantages of low cost, no pollution, the enhancement of product quality, and good application prospect.
Description
Technical field
The present invention relates to the xylan preparation field, be specifically related to a kind of preparation method of refining xylan.
Background technology
Xylan extensively is present in nature, accounts for the 20-30% of stalk dry weight, is the inexhaustible but carbohydrate demanding urgently developing of a class.People are that for the interest of xylan it is a renewable resources in one's early years, can replace grain to be used as fermentation raw material or animal-feed.Along with the reach of science, people's health care consciousness is constantly strengthened, and the demand of healthcare product is improved constantly; Current people's bigger interest is to have from the xylan preparation product such as xylo-oligosaccharide, wood sugar or Xylitol or the like of nourishing function.The xylo-oligosaccharide (2-7 wood sugar short chain) that is produced by xylan degrading is good functional oligose, compare with other oligose, xylo-oligosaccharide has better stability, can promote bifidus bacillus propagation in specificity ground, therefore, it is the most effective bifidus factor, only needs picked-up 0.7 gram just can reach whole intestines effect (general active oligose daily dosage portion is the 2-10 gram) for each person every day.The wood sugar that is produced by xylan hydrolysis can be hydrogenated and be reduced into Xylitol, and the sugariness of Xylitol is similar to sucrose with thermal capacity, is not subjected to Regular Insulin to control, can not be utilized, have by oral cavity bacterium characteristics such as anti-ketolysis but have metabolism.Therefore, the degraded product of xylan comprises xylo-oligosaccharide, wood sugar, Xylitol etc. at medicine, food etc., and industrial have a very big demand.
In the natural structure of plant, xylan and xylogen, Mierocrystalline cellulose closely combine, though xylan has the characteristic that can be dissolved in buck, and the certain degree of difficulty in addition of xylan being purified from other non-pentose constituents; Consider the purity of production cost, medicinal and edible product at needs, and during the problems such as offal treatment in the production process, it is especially complicated that the Separation ﹠ Purification technology of pentose series products seems.Because have chemical bond mutually crosslinked between xylan and xylogen, the xylan that obtain purifying is very difficult.But the xylan that has a small amount of xylogen can further be purified to remove and other material of its miscellaneous through after slightly extracting.
The thick extracting method of xylan commonly used is with aqueous slkali soaking and heating xylan to be extracted from plant fiber material; Centrifugal and regulate pH value back adding ethanol in alkali extract xylan etc. is precipitated out from the raw material extract, centrifugal again or filter to isolate and slightly carry xylan.
The process for purification of existing xylan is to be dissolved in water with slightly carrying xylan, adds 3 times of volume of ethanol again and makes the xylan precipitation and isolate xylan; Repeat the solubility small molecular weight impurity that several accompanies with macromole such as removal and xylans.Solvent load is big in this xylan process for purification, and the sewage of generation is many, and therefore the problem of cost height, blowdown difficulty is arranged; Also need to add oxygenants such as hydrogen peroxide or hypochlorite in the process for refining that has and make the goods color thin out, this not only increases operation and cost, and can produce the waste water that contains oxygenant.
In addition, the xylan raw product and the highly finished product that prepare with existing method structurally all are the agglutinating lumps, are difficult to drying, also are difficult to dissolving.Therefore, through after the oxidation of long period, product colour is very dark in drying process.
Summary of the invention
In order to overcome the deficiency of cost height among the existing xylan preparation method, generation sewage, the invention provides a kind of low cost, the extraction of free of contamination xylan, process for purification, on this basis, the also open method of further improving product quality of the present invention.
The technical scheme of technical solution problem of the present invention is as follows:
Steps A: go out alkali-soluble substance in the raw material with the alkaline solution extracting;
Step B: in the alkali extracted solution, add ethanol, use acid-conditioning solution pH behind the mixing; Centrifugal or filtration collecting precipitation thing is slightly carries xylan;
Step C: slightly carry xylan at least once with washing with alcohol, the throw out that obtains is the xylan of purification.
In the step B of technique scheme, regulate the pH value after adding ethanol earlier, can guarantee that the xylan flocculation is even, careful, can improve xylan output, reduce instrument burn into minimizing pigment, improve the color and luster of product, not only helped the structure quality that improves follow-up decontamination effect improving but also can improve product; Cause that easily some alkali extracted solution condense if regulate pH before adding ethanol, xylan granular size heterogeneity when adding ethanol again is difficult to purify.
Add the alcoholic acid amount among the inventive method step B, decide, when alcohol concn is low by concentration of ethanol and production cost, suitably increase the ethanol consumption, can improve sedimentation effect, it is 1-5 times of volume of alkali extracted solution that the present invention recommends the ethanol consumption, and alcohol concn is higher than 90% o'clock preferred 3 times of volume.
PH value described in the step B of the present invention is recommended 4-7, preferred 6.0.
Acid described in the step B of the present invention recommends to use phosphoric acid or sulfuric acid.After neutralization, do not use oxygenant also can obtain coloury product, and the final waste that produces can be made sulphur, phosphorus, potash fertilizer.
Ethanol described in the inventive method recommends working concentration to be equal to or higher than 75% ethanol, preferred ethanol more than 90%, preferably 95% ethanol.
The inventive method step C: slightly carry xylan at least once with washing with alcohol, the throw out that obtains is the xylan of purification.Wherein saidly slightly carry xylan with washing with alcohol and be meant, add ethanol in the xylan, throw out is smashed the back stirring at low speed make abundant balance to slightly carrying of being obtained, centrifugal or filter the collecting precipitation thing, remove the solubility small-molecule substance; Can improve the purity of product with the washing times increase, but the also corresponding increase of operation, the present invention recommends 2-5 time, and preferably working concentration is higher than 90% washing with alcohol 3 times.
Be used for thorough washing, dissolving in the scavenging process of the inventive method step C xylan attached to the micromolecular ethanol of the solubility on the xylan, can utilize once more, be introduced directly into the alkali extracted solution, slightly carry xylan in order to precipitate.
The extracting of alkali-soluble substance in the inventive method, adopt existing technology to get final product, but recommend following concrete operations: add the KOH or the NaOH aqueous solution that 3-10 rises 1%-5% in every kg feed material, soaked 2 hours to 2 days, boiling 15-30 minute, the solution of squeezing out; In residue, add a small amount of KOH or the NaOH aqueous solution again, boiling 15-30 minute once more, the solution of squeezing out.Merge two portions press juice, centrifugal or remove by filter throw out and be the alkali extracted solution.In order to reduce consumption of ethanol in the subsequent technique, the alkali extracted solution can preferably add the 1/2-1/5 that gentleness is evaporated to original volume through concentrating.
Raw material described in the inventive method recommends to select for use stalk class forage, corn cob or the bagasse that is rich in vegetable fibre.Before with the alkaline solution extracting, above-mentioned raw materials is carried out pre-treatment, can improve extraction rate was acquired, specifically be to wear into broken silk with the dust removal removal of impurities of stalk class forage and after drying, or corn cob worn into fragment, bagasse can be directly carry out next step buck extracting as raw material, and also available existing traditional technology mode is to raw material processing such as pulverize, sieve.
Strength of solution described in the present invention is if no specified otherwise all refers to weight ratio.
The general characteristic that application the inventive method prepares the technical process (Fig. 1) of xylan is dissolution characteristics and macromole and the difference of small-molecule substance aspect solubleness that has made full use of xylan, obtains the most approaching natural product with minimum chemical reagent and minimum procedure of processing.Realize that in conjunction with benefit and environmental requirement low consumption is pollution-free at aspects such as reagent type, solvent strength, reaction volumes.
Slightly carrying in the process of the xylan of recommending in the present invention adds in the alkali extracted solution behind the ethanol with phosphoric acid or sulphur acid for adjusting pH value.Its beneficial effect is:
(1) use the phosphorus acid for adjusting pH value, do not need when resulting xylan is used to prepare enzyme digestion reaction with damping fluid, the residuum of the supernatant liquor of generation after ethanol is reclaimed in distillation is the potassiumphosphate or the sodium radio-phosphate,P-32 solution of neutral meta-acid, can make farmland fertilizer and use;
(2) use the sulphur acid for adjusting pH value, resulting xylan color is pale yellow, that is to say with phosphoric acid, hydrochloric acid, acetic acid etc. and compare that sulfuric acid has tangible whitening effect; Be used with KOH, waste can be made potash fertilizer.
In the scavenging process of the xylan that the present invention recommends, with the precipitated xylan of high concentration ethanol thorough washing, its beneficial effect is:
(1) ethanol is amphoteric solvent, can fully dissolve attached to the solubility small molecules on the xylan, comprises water-soluble and fat-soluble small molecular weight impurity;
(2) use the high concentration ethanol thorough washing, the xylan that is flocculated is further dewatered, product structure is loose, is easy to drying, and color is light.
(3) high concentration ethanol is used for can being introduced directly into the alkali extracted solution behind the refining xylan, slightly carries xylan in order to precipitate, and therefore, the scavenging process of xylan does not consume reagent or solvent basically.
(4) whole process is workable, and the efficient height is suitable for a large amount of preparation xylans from agricultural wastes, for the production of xylo-oligosaccharide, wood sugar, Xylitol is supplied raw materials.
Description of drawings
Fig. 1 is the process flow diagram of preparation xylan;
Fig. 2 is that the HPLC of refining xylan analyzes collection of illustrative plates;
Fig. 3 is that the HPLC of xylanase hydrolysis liquid analyzes collection of illustrative plates;
Fig. 4 is that the HPLC of xylo-oligosaccharide analyzes collection of illustrative plates.
Embodiment
Further specify the inventive method below in conjunction with accompanying drawing:
Embodiment 1:
(1) nothing is gone mouldy straw shrug off dust and dry after wear into the long broken grass silk of 1-20mm;
(2) take by weighing grass silk 10kg, add 2.5% KOH solution 501, soaked extrusion solution 4 hours boiling 15-30 minute later on; In careless slag, add 201 2.5% KOH solution again, boiling 15-30 minute once more, extrusion solution.Merge two portions and extrude liquid, obtain supernatant liquor about 501 at the centrifugal 30min of centrifugal force 8000g;
(3) add 95% ethanol 150L, with phosphorus acid for adjusting pH value to 6.0,, collect the precipitated xylan of slightly carrying behind the mixing in the centrifugal 15min of 8000g;
(4) the ethanol 50l of adding 95% in slightly carrying xylan precipitation piece smashes the back stirring at low speed and made its abundant balance in 2 hours, in the centrifugal 15min collecting precipitation of 8000g thing; Add ethanol again and repeat aforementioned process 2 times, obtain product, get product sample and analyze as shown in Figure 2, wherein HPLC analytical column: Sugarpak 1 through HPLC; 6.5mm the analysis of * 300mm sugar post, chromatographic condition: column temperature: 85 ℃; Moving phase: water; Flow velocity: 0.5mL/min; Differential refraction detector sensitivity: 4, external standard method is demarcated, and sample size is 10 μ L.Standard model is purchased the company in Sigma, and according to standard specimen, peak 14.0 is a wood sugar.
Embodiment 2: substantially the same manner as Example 1, difference is the broken wheat straw with 10kg, and the NaOH solution of 30L1%, 80% ethanol 50L slightly carry xylan;
Embodiment 3: substantially the same manner as Example 1, difference is that the KOH solution of making raw material, 100L5% with 10kg bagasse extracts alkali-soluble substance, gets alkali extract 80L, and reconcentration is to 40L; Add 85% ethanol 200L then and slightly carry xylan.
Embodiment 4: substantially the same manner as Example 1, difference is with sulphur acid for adjusting pH value to 4.
Embodiment 5: substantially the same manner as Example 1, difference is with acetate the pH value to be transferred to 7.
Embodiment 6: substantially the same manner as Example 1, difference is slightly to carry xylan with 70% ethanol 301 purifications, repeats 4 times.
Embodiment 7: substantially the same manner as Example 1, difference is that 75% ethanol 201 purifies and slightly carries xylan, repeats 6 times.
Embodiment 8: substantially the same manner as Example 1, difference is that 90% ethanol 401 purifies and slightly carries xylan 3 times.
Embodiment 9: substantially the same manner as Example 1, difference is that (1) wherein, the step that (2) produce alkali extracting solution substitute with existing technology.
Embodiment 10: the product that obtains with embodiment 1 is a raw material, method with reference to Chinese patent 200410064667.4 prepares xylo-oligosaccharide, analyze xylanase hydrolysis liquid and remove the xylo-oligosaccharide that undecomposed composition obtains with HPLC, the result distinguishes as shown in Figure 3, Figure 4, and the HPLC analysis condition is with embodiment 1.Show the product precision height that the present invention makes, quality better.
Claims (10)
1, a kind of method for preparing refining xylan, its steps in sequence is as follows:
Steps A: go out alkali-soluble substance in the lignocellulose raw material with the alkaline solution extracting;
Step B: in the alkali extracted solution, add ethanol, use acid-conditioning solution pH behind the mixing; Centrifugal or filtration collecting precipitation thing is slightly carries xylan;
Step C: slightly carry xylan at least once with washing with alcohol, the throw out that obtains is the xylan of purification.
2, xylan preparation method according to claim 1 is characterized in that, and is described
Step B is: in the alkali extracted solution, add 1-5 times of volume of ethanol, behind the mixing with acid for adjusting pH to 4-7; Throw out centrifugal or that filtration is collected is slightly carries xylan.
3, xylan preparation method according to claim 2 is characterized in that, adds 3 times of volume of ethanol among the described step B in the alkali extracted solution.
4, xylan preparation method according to claim 3 is characterized in that, the acid described in the step B is phosphoric acid or sulfuric acid.
According to the described xylan preparation method of one of claim 1-4, it is characterized in that 5, described ethanol is that concentration is equal to or higher than 75% ethanol.
6, xylan preparation method according to claim 5 is characterized in that, described alcohol concn is 90-95%.
7, xylan preparation method according to claim 5 is characterized in that, is equal to or higher than 75% washing with alcohol with concentration among the described step C and slightly proposes xylan 2-5 time.
8, xylan preparation method according to claim 7 is characterized in that concrete operations are as follows:
Steps A: add the KOH or the NaOH aqueous solution that 3-10 rises 1%-5% in every kg feed material, soaked 2 hours to 2 days, boiling 15-30 minute, the solution of squeezing out; Add a small amount of KOH or the NaOH aqueous solution in residue again, boiling 15-30 minute once more, the solution of squeezing out merged two portions press juice, and is centrifugal or remove by filter throw out and be the alkali extracted solution;
Step B: in the alkali extracted solution, add 95% ethanol of 3 times of volumes, regulate pH to 6.0 with phosphoric acid behind the mixing; Throw out centrifugal or that filtration is collected is slightly carries xylan;
Step C: add 95% ethanol in the xylan to slightly carrying, smash the back stirring at low speed and make abundant balance, centrifugal or filtration collecting precipitation thing; Repeat this process 2 times, obtain xylan.
9, according to the described xylan preparation method of one of claim 1-4, it is characterized in that also having following process between steps A and B: the alkali extract that steps A is obtained concentrates.
10, xylan preparation method according to claim 5 is characterized in that, washs the ethanol of slightly carrying xylan among the step C and is used to step B.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN 200510039239 CN1283649C (en) | 2005-05-10 | 2005-05-10 | Preparation method of refining xylan |
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| CN 200510039239 CN1283649C (en) | 2005-05-10 | 2005-05-10 | Preparation method of refining xylan |
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| CN1283649C true CN1283649C (en) | 2006-11-08 |
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| CN 200510039239 Expired - Fee Related CN1283649C (en) | 2005-05-10 | 2005-05-10 | Preparation method of refining xylan |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FI126212B (en) * | 2012-03-27 | 2016-08-15 | Upm Kymmene Corp | Process and system for isolating xylan from plant material |
| CA2987869C (en) * | 2015-06-10 | 2023-03-28 | Stora Enso Oyj | Methods for treating lignocellulosic materials |
| CN106674382A (en) * | 2017-01-13 | 2017-05-17 | 河南工业大学 | Method for extracting high-purity xylan from pawpaw fruits |
| CN108720030B (en) * | 2018-05-11 | 2021-12-14 | 广西壮族自治区中国科学院广西植物研究所 | Dietary fiber composition for targeted improvement of metabolic syndrome |
| CN108359026B (en) * | 2018-05-11 | 2021-04-27 | 唐传生物科技（厦门）有限公司 | Preparation method and application of water-insoluble xylan |
| CN109160961A (en) * | 2018-09-05 | 2019-01-08 | 北华大学 | A kind of Nano xylan and its preparation method and application |
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