CN111019015B - Preparation method of high-purity water-insoluble xylan - Google Patents
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Abstract
The invention discloses a preparation method of high-purity water-insoluble xylan, which comprises the steps of preparing xylan extraction alkali liquor by using stems and leaves of gramineous plants, obtaining lignin-containing xylan suspension through dealkalization treatment, then heating and drying to prepare xylan xerogel with slow rehydration, dissolving the lignin which is hydrolyzed slowly and quickly in water by using the property difference that the xylan xerogel is slow in rehydration swelling process and is dissolved quickly in alkaline water, crushing the xylan xerogel, and then putting the crushed xylan xerogel into flowing purified water for rinsing, so that the embedded lignin is fully removed before the xylan gel is fully swelled and crushed, and the high-purity water-insoluble xylan is obtained. The preparation method of the invention does not use organic solvent, effectively reduces the production cost, is easy to obtain high-purity xylan products, can recover high-purity lignin products, and has good economy, feasibility and production safety.
Description
Technical Field
The invention belongs to the field of food science, and particularly relates to a preparation method of high-purity water-insoluble xylan.
Background
Xylan is a main component of hemicellulose of a cell wall of a gramineous plant, accounts for about 1/3 in dry weight of the cell wall, and is a polysaccharide in which several tens to several hundreds of xylose molecules are linked in beta- (1 → 4) to constitute a main chain. The 2,3C of xylan backbone sugar groups typically also link heterogeneous glycans with different sugar-based and non-sugar substituent branches. Xylan is the only pentose polymer in the nature, and the unique performance of xylan has irreplaceable application value in the fields of food, chemical industry and the like.
Xylans in plant cell walls are highly acetylated and become strong support materials for plant cell walls by ester bonds in combination with lignin. Hydrolysis with alkali removes acetyl groups, breaking the ester bonds to lignin, and xylans will dissociate from the plant cell wall and go into solution. At the same time, the alkali can also catalyze the depolymerization of insoluble lignin high polymers of plant cell walls to generate water-soluble low-molecular-weight lignin. Therefore, the process of extracting xylan with alkali liquor is the process of dissolving xylan in plant raw materials with alkali liquor, depolymerizing macromolecular lignin, separating xylan and soluble lignin with low polymerization degree from the alkali liquor, and respectively recovering. The lignin with low degree of polymerization dissolved in the alkali liquor can be dissolved in ethanol, and the xylan is not dissolved in the ethanol, so that the ethanol precipitation method is the most commonly used xylan-lignin separation method by utilizing the difference of chemical properties. However, the process for separating xylan by ethanol precipitation not only has high solvent consumption cost, but also is difficult to apply to large-scale industrial production of xylan.
The solubility of xylan is determined by the number of branched substituents, with higher number of substituents, i.e. higher degree of substitution, giving better water solubility. The degree of substitution of xylan branches is related to the plant origin, the parts of plant organs. The branched chain substitution degree of xylan at grain parts (such as wheat bran, rice bran and corn bran) of the gramineous crops is high, the water solubility is taken as the main point, but the branched chain substitution degree of the straw xylan is low, so most of the straw xylan is difficult to dissolve in water, but can disperse the water to form a relatively stable suspension. The characteristics of insoluble xylan have application value irreplaceable to water-soluble xylan, but it is not easy to realize the economic preparation of pure insoluble xylan.
The xylan suspension can be separated from the lignin solution by membrane filtration or centrifugation. The present applicant has disclosed in patent application No. 201810446453.5 a method for preparing water-insoluble xylan: extracting xylan from plant cell wall with alkali solution, ultrafiltering to eliminate most of alkali solution, precipitating xylan, replacing and ultrafiltering with dilute alkali solution for several times to eliminate lignin, and washing with centrifugal or micro-filtering membrane to obtain xylan with purity up to 85-90%. Alcohol is not used in the whole process, and only water-insoluble xylan, lignin and other soluble impurities in the product are completely removed. However, the separation and purification efficiency of displacement ultrafiltration and displacement microfiltration is not high in nature, and xylan gel particles are also accumulated on the surface of the filter membrane to form a dense gel filtration layer, which seriously affects the filtration efficiency of the membrane. The method for obtaining pure xylan by removing lignin by using a membrane filtration method has high cost and is difficult to realize large-scale industrial production of xylan.
Disclosure of Invention
In order to solve the defects in the prior art, the invention aims to provide the preparation method of the high-purity water-insoluble xylan, which does not use an organic solvent, greatly saves the use cost of the organic solvent, effectively avoids the flammable and explosive risks caused by using a large amount of the organic solvent, is easy to obtain a high-purity xylan product, can recover a high-purity lignin product, and has good economy, feasibility and production safety.
A method for preparing high-purity water-insoluble xylan comprises the following steps:
(1) cleaning and dehydrating stems and leaves of gramineous plants without mildew, adding 5-15 times volume of 3-20% sodium hydroxide or potassium hydroxide solution, leaching at 60-90 deg.C for 2.5-3.5 hr, performing solid-liquid separation, adding 5-15 times volume of 3-20% sodium hydroxide or potassium hydroxide solution into the residue, leaching at 60-90 deg.C for 2.5-3.5 hr until lignin high polymer in the raw material depolymerizes and xylan is sufficiently deacetylated and dissolved in alkali liquor, recovering and combining the liquid phase parts of the two leachates, and clarifying to obtain xylan leaching alkali liquor.
(2) And (3) carrying out dealkalization treatment on the xylan extraction alkali liquor, recovering alkali in the xylan extraction alkali liquor, neutralizing residual alkali in the dealkalized extraction liquor by using acid, and adjusting the pH value to 7-9 to obtain a lignin-containing xylan suspension.
(3) And concentrating the xylan suspension, and then heating, dehydrating and drying to obtain xylan xerogel with the water content of less than 25%.
(4) And crushing the xylan xerogel to obtain xylan gel powder, pre-swelling the xylan gel powder by using clear water, and rinsing the xylan gel powder in flowing purified water to remove lignin to obtain the pure xylan gel.
(5) And dehydrating and drying the pure xylan gel to obtain high-purity water-insoluble xylan, and concentrating and drying the rinsing solution to obtain a lignin product.
The dealkalization treatment method in the step (2) is the existing conventional dealkalization treatment method, and can be electrodialysis, diffusion dialysis, ultrafiltration, nanofiltration or acid neutralization, but is not limited to the methods.
And (4) the dehydration drying in the step (3) or the step (4) is drying by using a spray dryer, a drum dryer, a flash dryer, a boiling dryer, a vacuum dryer or a spiral dryer and the like.
The rinsing in the step (4) can adopt a vertical column fluidization washing mode or a horizontal pipe type countercurrent washing mode.
The gramineous plants include wheat straw, bagasse or leaves, rice straw, miscanthus, corn stalks, corn cobs, sorghum, bamboo, thatch and the like.
Preferably, the rinsing in the step (4) by adopting the vertical columnar fluidized washing mode is to crush the xylan xerogel, pre-swell the crushed xylan xerogel by using clear water, immediately put the crushed xylan xerogel into a washing column which is filled with clear water in advance, continuously and slowly introduce the clear water into the bottom of the washing column to maintain the xylan gel particles to sink at the bottom of the washing column, and the lignin leaves the washing column from an overflow port at the top of the column along with water flow and is collected as rinsing liquid. When the rinsing liquid is colorless, the lignin in the xylan gel particles is removed, and the rinsing process is finished.
Preferably, the step (4) of rinsing by adopting a transverse pipe type countercurrent washing mode is to crush xylan xerogel, pre-swell the crushed xylan xerogel by using clear water, immediately put one end of the crushed xylan xerogel into a transverse pipe washing column which is filled with clear water in advance, continuously and slowly feed the clear water into the other end of the washing column, push xylan gel particles to the injection end of the clear water through a transmission screw, and leave the washing pipe from the overflow port of the feeding end along with water flow and collect lignin. When the xylan gel particles pass through the clean water injection end and the rinsing liquid at the rear section of the clean water injection end is colorless, the lignin in the xylan gel particles is removed, and the rinsing process is finished.
The invention has the beneficial effects that:
1. in the invention, the separation and purification process of the water-insoluble xylan completely abandons organic solvents, and the safety, the economy and the environmental friendliness of the industrial production process are incomparable with those of the traditional organic solvent precipitation separation process. Drying can break the emulsion state of water-insoluble xylan and lignin in water phase, the water-insoluble xylan in the xylan xerogel is hardened and aggregated in water and is not easy to disperse, and the lignin depolymerized by alkali is dissolved in water. Therefore, the invention firstly heats and dries the lignin-containing xylan suspension to prepare the xylan xerogel with slow rehydration, and then fully removes the embedded lignin before the xylan gel is fully swelled and broken by only rinsing with running water by utilizing the important property difference that the xylan xerogel is slow in rehydration and swells and the lignin hydrolyzed by alkali is quickly dissolved by water. Compared with the traditional organic solvent precipitation method, the method has the advantages that the xylan must be repeatedly washed by the solvent to remove the lignin and obtain a pure xylan product, the process of the invention not only greatly saves the use cost of the organic solvent, but also effectively avoids the flammable and explosive risks brought by using a large amount of the organic solvent, and has good economy, feasibility and production safety.
2. Under the condition of the same separation cost, the purity of the xylan obtained by the method is far higher than that of xylan prepared by other separation methods, and the method has wider application fields and higher commercial value. The xylan xerogel prepared by the invention continuously absorbs water to swell, and lignin in the xylan xerogel can be dissolved out from the xylan gel particles more easily. And the organic solvent is used for precipitating xylan, so that lignin entrained by xylan precipitate is continuously dehydrated, aggregated and compacted, and the lignin is more and more difficult to diffuse and displace from the xylan precipitate. Obviously, the separation mechanism adopted by the invention can easily obtain the high-purity xylan product, while the organic solvent precipitation method has more difficulty in obtaining the xylan product with the same purity and is difficult to obtain the xylan product with very high purity. The xylan content in the water-insoluble xylan product obtained by the method reaches more than 85 percent, and the requirement of food and medical industries on the purity of the xylan product can be easily met, which is difficult to realize by the traditional process; the method can also recover lignin products, and the lignin content in the products reaches more than 60 percent.
Drawings
FIG. 1 is a high performance liquid chromatogram of a water-insoluble xylan standard (2 g/L);
FIG. 2 is a high performance liquid chromatogram of the water-insoluble xylan product of example 1;
FIG. 3 is a high performance liquid chromatogram of the water-insoluble xylan product of example 2;
FIG. 4 is a high performance liquid chromatogram of the water-insoluble xylan product of example 3.
Detailed Description
In order to describe the present invention in more detail, the present invention will be further described with reference to the following examples.
Example 1
A method for preparing high-purity water-insoluble xylan comprises the following steps:
(1) weighing 10kg of mildew-free air-dried bagasse, washing with clear water for 2 times, centrifugally dewatering, and putting into a reaction kettle.
(2) Adding 100kg of sodium hydroxide solution with the mass concentration of 14%, heating to 60 ℃, leaching for 3 hours, and carrying out solid-liquid separation after leaching.
(3) The residue after solid-liquid separation was repeatedly leached once with 50kg of 8% sodium hydroxide solution, and solid-liquid separation was performed again.
(4) Mixing the two extracted alkali liquors, filtering with plate-frame filter, concentrating, removing alkali with alkali-resistant ultrafiltration membrane, ultrafiltering twice with water until a small amount of xylan is precipitated to obtain alkali-removed extract, and recovering alkali liquor. The recovered alkali liquor can be reused for leaching air-dried bagasse, so that the recycling rate of the sodium hydroxide solution is improved, and the cost of the alkali liquor is reduced.
(5) Neutralizing the dealkalized leaching solution by hydrochloric acid until the pH value is 10 to obtain lignin-containing xylan suspension.
(6) And concentrating the xylan suspension by proper alkali pressure, and then performing spray drying to obtain xylan gel powder, wherein the water content of the gel powder is less than 10%.
(7) Pre-swelling xylan gel powder with clear water, immediately putting into a washing column filled with clear water in advance, continuously and slowly introducing clear water into the bottom of the washing column, keeping xylan gel particles settled at the bottom of the washing column, and collecting lignin as rinsing liquid after the lignin leaves the washing column from an overflow port at the top of the column along with water flow. When the rinsing liquid is colorless, the lignin in the xylan gel particles is removed, and the rinsing process is finished.
(8) Grinding the rinsed xylan gel particles by a colloid mill until the particle size is less than or equal to 0.1mm and the size is uniform, and then drying by a spray dryer; concentrating the collected lignin rinsing liquid in vacuum, and drying by using a spray dryer; the air inlet temperature of the spray drying is set to be 120-300 ℃, and the air outlet temperature is more than 75 ℃.
Example 2
A method for preparing high-purity water-insoluble xylan comprises the following steps:
(1) weighing 10kg of mildew-free air-dried bagasse, washing with clear water for 2 times, centrifugally dewatering, and putting into a reaction kettle.
(2) Adding 100kg of sodium hydroxide solution with the mass concentration of 14%, heating to 60 ℃, leaching for 3 hours, and carrying out solid-liquid separation after leaching.
(3) The residue after solid-liquid separation was repeatedly leached once with 50kg of 8% sodium hydroxide solution, and solid-liquid separation was performed again.
(4) Mixing the two extracted alkali liquors, filtering with plate-frame filter, concentrating, removing alkali with alkali-resistant ultrafiltration membrane, ultrafiltering twice with water until a small amount of xylan is precipitated to obtain alkali-removed extract, and recovering alkali liquor. The recovered alkali liquor can be reused for leaching air-dried bagasse, so that the recycling rate of the sodium hydroxide solution is improved, and the cost of the alkali liquor is reduced.
(5) Neutralizing the dealkalized leaching solution by hydrochloric acid until the pH value is 10 to obtain lignin-containing xylan suspension.
(6) Concentrating the xylan suspension by proper alkali pressure, and drying by a roller to obtain a xylan gel sheet-like dried substance and dry powder, wherein the water content is less than 10%.
(7) The method comprises the following steps of crushing xylan gel sheets properly, pre-swelling dry powder with clear water, putting the crushed dry powder into a horizontal pipe washing column filled with clear water in advance at one end, continuously and slowly introducing clear water into the other end of the washing column, pushing xylan gel particles to the injection end of the clear water through a transmission screw, and collecting lignin which leaves a washing pipe from an overflow port of a feeding end along with water flow. When the xylan gel particles pass through the clean water injection end and the rinsing liquid at the rear section of the clean water injection end is colorless, the lignin in the xylan gel particles is removed, and the rinsing process is finished.
(8) Grinding the rinsed xylan gel particles by a colloid mill until the particle size is less than or equal to 0.1mm and the size is uniform, and then drying by a spray dryer; concentrating the collected lignin rinsing liquid in vacuum, and drying by using a spray dryer; the air inlet temperature of the spray drying is set to be 120-300 ℃, and the air outlet temperature is more than 75 ℃.
Example 3
A method for preparing high-purity water-insoluble xylan comprises the following steps:
(1) weighing 10kg of mildewless air-dried corncobs, washing with clear water for 2 times, dewatering by using a vibrating screen, shredding by using a double-shaft shredder for 2 times to obtain corncob small particles, and putting the corncob small particles into a reaction kettle.
(2) Adding 100kg of sodium hydroxide solution with the mass concentration of 14%, heating to 60 ℃, leaching for 3 hours, and carrying out solid-liquid separation after leaching.
(3) The residue after solid-liquid separation was repeatedly leached once with 50kg of 8% sodium hydroxide solution, and solid-liquid separation was performed again.
(4) Mixing the two extracted alkali liquors, filtering with plate-frame filter, concentrating, removing alkali with alkali-resistant ultrafiltration membrane, ultrafiltering twice with water until a small amount of xylan is precipitated to obtain alkali-removed extract, and recovering alkali liquor. The recovered alkali liquor can be reused for leaching the air-dried small corn cob particles, so that the recycling rate of the sodium hydroxide solution is improved, and the cost of the alkali liquor is reduced.
(5) Neutralizing the dealkalized leaching solution by hydrochloric acid until the pH value is 10 to obtain lignin-containing xylan suspension.
(6) After the xylan suspension is properly decompressed and concentrated, the xylan gel powder is obtained by spray drying, and the water content of the gel powder is less than 10%.
(7) Pre-swelling xylan gel powder with clear water, immediately putting into a washing column filled with clear water in advance, continuously and slowly introducing clear water into the column bottom, keeping xylan gel particles settled at the bottom of the washing column, and collecting lignin as rinsing liquid after lignin leaves the washing column from an overflow port at the column top along with water flow. When the rinsing liquid is colorless, the lignin in the xylan gel particles is removed, and the rinsing process is finished.
(8) Grinding the rinsed xylan gel particles by a colloid mill until the particle size is less than or equal to 0.1mm and the size is uniform, and then drying by a spray dryer; concentrating the collected lignin rinsing liquid in vacuum, and drying by using a spray dryer; the air inlet temperature of the spray drying is set to be 120-300 ℃, and the air outlet temperature is more than 75 ℃.
The invention detects the water-insoluble xylan product and lignin product prepared by the embodiment: HPLC method is adopted to determine total glycan content, ultraviolet spectrophotometry method is adopted to determine lignin content, moisture and ash content are respectively determined according to standards GB/T5009.3 and GB/T5009.4, DNS method is adopted to determine water-soluble reducing sugar content in xylan, detection results are shown in tables 1 and 2, and high performance liquid chromatogram of water-insoluble xylan products and water-insoluble xylan standard products (2 g/L) in examples 1-3 are shown in figures 1-4.
Claims (3)
1. A method for preparing high-purity water-insoluble xylan, comprising the steps of:
(1) crushing, cleaning and dehydrating stems and leaves of gramineous plants without mildew, adding 5-15 times of sodium hydroxide or potassium hydroxide solution with the mass concentration of 3-20%, leaching for 2.5-3.5h at 60-90 ℃, carrying out solid-liquid separation, adding 5-15 times of sodium hydroxide or potassium hydroxide solution with the mass concentration of 3-20% into residues again, leaching for 2.5-3.5h at 60-90 ℃ until lignin high polymer in the raw materials is depolymerized and xylan is sufficiently deacetylated and dissolved into alkali liquor, finishing leaching, then carrying out solid-liquid separation, recovering and combining liquid phase parts obtained by two times of leaching, and clarifying to obtain xylan leaching alkali liquor;
(2) carrying out dealkalization treatment on xylan extraction alkali liquor, recovering alkali in the xylan extraction alkali liquor, neutralizing residual alkali in the dealkalized extraction liquor with acid, and adjusting the pH value to 10 to obtain lignin-containing xylan suspension;
(3) concentrating the xylan suspension, heating for dehydration and drying to obtain xylan xerogel;
(4) crushing the xylan xerogel to obtain xylan gel powder, pre-swelling the xylan gel powder by using clear water, and then putting the xylan gel powder into flowing purified water for rinsing to remove lignin to obtain pure xylan gel; the rinsing adopts a vertical columnar fluidization washing mode or a horizontal tubular countercurrent washing mode;
(5) and dehydrating and drying the pure xylan gel to obtain high-purity water-insoluble xylan, and concentrating and drying the rinsing liquid to obtain a lignin product.
2. The method for preparing high-purity water-insoluble xylan according to claim 1, wherein the dealkalizing treatment of step (2) is electrodialysis, diffusion dialysis, ultrafiltration, or nanofiltration.
3. The method for producing a high-purity water-insoluble xylan according to claim 1, wherein the dehydration drying in step (3) or step (5) is drying using a spray dryer, a drum dryer, a flash dryer, a boiling dryer, a vacuum dryer, or a screw dryer.
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