KR100638607B1 - The production method for xylose maked from bamboos - Google Patents

Abstract

A method for producing xylose by using a bamboo is provided to collect xylose generated as a by-product in a pulp manufacturing process and make use of the xylose as resources, thereby efficiently utilizing natural resources. Leafs are removed from a bamboo. The bamboo is slit vertically by cutting at a gap of 1.5-3 mm. Bamboo chips are produced by horizontally cutting the vertically cut bamboo in length of 10-30 mm. The cut bamboo chips are screened to filter scraps or impurities. Impurities, alien substance and dust of the bamboo chips are cleaned. The bamboo chips are pre-hydrolyzed to elute hemicellurose, wherein a catalyst is added according to required reaction of pre-hydrolysis for stimulating pre-hydrolysis. The bamboo chips are put into a digester to be digest at a high temperature at a mixture of bamboo and a medical fluid consisting of water, alkali and anthraquinone in a ratio of 1:3.5-6.0 so that the bamboo chips are soften to be made into pulp. Carbonic acid gas is supplied for neutralization and deposition to elute xylose. A mixture of water, alcohol and methyl isobutyl ketone is added to separate a phase while controlling a rate of water. Alcohol is added to the separated aqueous solution for precipitating xylose.

Description

The production method for xylose maked from bamboos}

The present invention relates to a method for manufacturing xylose using bamboo, in particular, to solve the economic and environmental problems of the prior art as well as eluting in the pre-hydrolysis process and cooking process in the process of producing high-quality dissolving pulp. The present invention relates to a method for producing xylose using bamboo for recovering and recycling xylose from hemicellulose which is to be produced.

Until recently, xylose is mainly produced from birch. In addition, a method of separating xylose from eluted components by cooking various woods or herbs with organic solvents is also used.

Since these methods produce only xylose from raw materials, they are very disadvantageous in terms of efficient use of resources and economics, and contribute to the high price of xylose.

In addition, unbleached and bleached chemical pulp prepared by various methods may be acid hydrolyzed, or xylose may be produced from pulp through alkali extraction and enzyme treatment.

All of these methods are mainly focused on the production of xylose. Therefore, considering the current situation in which various deregulations and movements are being conducted to reduce greenhouse gases and protect the global environment due to the worsening of the environment, whether or not the resource is effectively used as described above. Not only is not preferable in terms of economics but also in terms of economics.

Although some xylose is recovered from the cooking liquor from the wood-melting pulp manufacturing process, as the pressure on forest preservation intensifies, not only is it difficult to produce sufficient quantities, but the situation will worsen over time. There is no choice but to.

The present invention relates to a method for manufacturing xylose using bamboo, in particular, to solve the economic and environmental problems of the prior art as well as eluting in the pre-hydrolysis process and cooking process in the process of producing high-quality dissolving pulp. It is intended to provide a xylose production method that is produced using bamboo to recover and recycle xylose from the hemicellulose to be.

Therefore, the present invention provides a method for producing xylose produced using bamboo, the first step: removing the bamboo leaves to remove the leaves from the bamboo; Second step: vertical cutting to split the bamboo but cut vertically at intervals of 1.5-3 mm; A third step: a cutting step of producing a bamboo chip by cutting horizontally cut bamboo to a length of 10-30 mm; A fourth step: screening to filter debris or impurities from the cut bamboo chips; The fifth step: a washing step of washing impurities, foreign matters and dusts, etc., deposited on the bamboo chips with water; Step 6: Pre-hydrolysis step of washing washed bamboo chips using water or steam for pre-hydrolysis, and adding catalyst to promote pre-hydrolysis according to the required degree of pre-hydrolysis to dissolve hemicellulose Wow; Step 7: concentrating the solution separated from the bamboo chips through a heat exchange system or waste heat; Step 8: adding 50-150% of methanol, ethanol, a mixture of methanol and ethanol to the concentrated solution and precipitating xylose by alkanol precipitation; Step 9: separating the precipitated xylose by filtration or centrifugation; The tenth step: a step of refining through the treatment of acid hydrolysis; to provide a method for producing xylose produced by using bamboo to produce xylose, which is a raw material of gum.

In another aspect, the present invention provides a method for producing xylose produced using bamboo, the first step: removing the bamboo leaves to remove the leaves from the bamboo; Second step: vertical cutting to split the bamboo but cut vertically at intervals of 1.5-3 mm; A third step: a cutting step of producing bamboo chips by cutting horizontally cut bamboo to a length of 10-30 mm; A fourth step: screening to filter debris or impurities from the cut bamboo chips; The fifth step: a washing step of washing impurities, foreign matters and dusts, etc., deposited on the bamboo chips with water; Step 6: Pre-hydrolysis step in which washed bamboo chips are carried out using water or steam for prehydrolysis, and the catalyst is added according to the required degree of prehydrolysis to promote prehydrolysis to dissolve hemicellulose. Wow; Step 7: The bamboo chip is administered to the cooking section (Digester), and the ratio of the chemical weight consisting of water, alkali, and anthraquinone to the bamboo weight is 1: 3.5-6.0 (bamboo: chemical solution). A cooking step of pulping by softening the bamboo chips by cooking; Eighth step: neutralizing precipitate by supplying carbon dioxide gas to elute xylose; Step 9: adding water, alcohol, methyl isobutyl ketone mixture and phase separation while controlling the proportion of water in a well mixed state; Step 10: Precipitating xylose by adding alcohol to the separated aqueous solution; It is intended to provide a method for producing xylose produced by using bamboo to produce xylose, which is made of gum.

The present invention is similar to the conventional one in that the pulp is produced.

However, the present invention is to produce xylose using a non-wood plant bamboo, to extract xylose in the stage of pre-hydrolysis and cooking during the production of pulp, and thus do not have to lumber the wood present on earth This step is described in detail as there is a significant effect in the effect and the remarkable quality of the xylose made of bamboo.

In the present invention, the method for producing a dissolving pulp produced using bamboo, the first step: the step of removing the bamboo leaves to remove the leaves from the bamboo.

In other words, bamboo leaves have many extracts that are unnecessary to make pulp, while having less substantial fiber.

Therefore, the leaves are removed before entering the production process for dissolving pulp because they are likely to act to increase the consumption of the chemical rather than to help the production of pulp.

That is, in the method for producing bamboo pulp of the present invention, bamboo leaves are not used, but only bamboo Taiwan is used.

Next, the second step: split the bamboo, but goes through the vertical split (splitting) step to cut at a vertical interval of 1.5-3mm.

Bamboo is considerably more difficult to penetrate than wood because of its dense structural properties.

Therefore, it is necessary to grind to start the production of pulp. First, the split bamboo is cut into narrow widths while being split in half in the longitudinal direction of the bamboo.

At this time, the width of the bamboo is preferably cut to a width of 1.5-3mm.

This longitudinal cutting is a process that is quite characteristic in the present invention, if the bamboo is cut in a state ignoring random direction, there is a possibility that the phenomenon that the fiber itself is destroyed rather than uniformly cut the fiber produced.

Therefore, the strength of the produced pulp is weakened, the quality level is also lowered.

As a result, in the production method of the present invention is used to cut bamboo vertically many times to have a narrow width.

Of course, it is also possible to use a method of chopping bamboo at a time using a device equipped with multiple blades.

Thereafter, the third step: a longitudinal cutting of the vertically cut bamboo to a length of 10-30mm undergoes a cutting step to produce a bamboo chip.

In other words, in order to produce a small form of bamboo chips to be easy to fill and pack in the cooking section (digest) is cut to a length of 10-30mm horizontally using a cutter.

If the length of the bamboo chip is too long, it may not be efficiently packed in the cooking part (digest), while if cut too short, the damage of the fiber may occur, resulting in a weak pulp strength.

Next, the fourth step: the screening (screening) to filter the debris or impurities from the cut bamboo chip.

In other words, the debris generated in the process of cutting bamboo, even if made of pulp, the fiber is destroyed, so as not only to weaken the strength of the pulp but also increase the consumption of chemicals.

In addition, foreign materials introduced during the cutting process do not help the production of pulp.

Therefore, if all of them are used for the use of pulp, not only does it contribute to the yield of pulp (the yield of pulp obtained), but it is also harmful to the quality of the pulp.

Next, the fifth step: a washing step of washing impurities, foreign matter and dust on the bamboo chip with water.

That is, remove foreign substances, dust, and the like on the bamboo chip with water.

This reduces the consumption of unnecessary chemicals in the cooking process and also makes it possible to obtain pure pulp, which in turn improves the quality of the pulp produced.

Step 6: After washing the washed bamboo chip with water or steam for prehydrolysis, add the catalyst according to the required degree of prehydrolysis to promote prehydrolysis to dissolve the hemicellulose Go through the steps

That is, hydrolysis is performed to elute hemicellulose while maximizing the yield of pulp for dissolution in bamboo chips.

For this hydrolysis, hydrolysis is generally performed with liquid water or steam, and sulfuric acid or the like is used as the catalyst.

More precisely, sulfuric acid, hydrochloric acid, sulfurous acid and formic acid may be selectively applied and used.

The purpose of this pre-hydrolysis is to dissolve the hemicellulose in the bamboo chip, so if the acid is used alone, the acid hydrolysis may occur so severely that the cellulose may be severely destroyed.

Therefore, the ratio should be adjusted and used according to the working conditions.

Here, the liquid ratio, that is, the administration of the liquid water and the catalyst, and the administration ratio of the bamboo chip is preferably adjusted within the range of 1.5-7: 1 according to the degree of hydrolysis required.

In other words, the hydrolysis of the liquid containing water and the bamboo chip is 1.5-7: 1.

It should be noted that during the prehydrolysis, organic acids are generated as hemicellulose is decomposed in the chemical composition constituting bamboo, and the organic acids lead the hydrolysis of bamboo.

Therefore, the higher the liquid ratio is to be controlled according to the degree of polymerization, the degree of hydrolysis of hemicellulose using the characteristics of the hydrolysis proceeds slowly.

In other words, the liquid ratio (liquor ratio) is a bamboo chip (oven dry weight) is 1 when the volume of the aqueous solution (if the drug is dissolved in water if the drug, such as a catalyst) is 1.5-7 will be.

And the purpose of forming the liquid ratio is, first, to make the contact well with the chemical liquid during the reaction of the bamboo chip, the second, the strength (concentration) of the chemical liquid in contact with the bamboo chip according to the degree of liquid ratio By varying, the degree of reaction is controlled.

In addition, a slight difference may occur depending on the quality required for the decomposition conditions in this prehydrolysis step, but the temperature is set at 90-150 ° C., and the time for hydrolysis is controlled within a time range of 60-250 minutes. This is preferable.

Of course, these conditions have been proved through the applicant's many experiments.

In addition, there is a phrase "the whole thing" means that the bamboo chip contains a lot of moisture, which means the mass of pure bamboo chips except the moisture.

In addition, to calculate this yield, the moisture content of the bamboo chips is measured, and inversely, the weight of pure bamboo chips is calculated.

Next, the seventh step is concentrated through a heat exchange system or waste heat.

In other words, the temperature is raised and concentrated in the direction of blowing water vapor.

In addition, the next step, step 8: methanol, ethanol, a mixture of methanol and ethanol is optionally added to the concentrated solution 50-150% compared to the solution is subjected to the step of precipitating xylose by alkanol precipitation.

Step 9: The precipitated xylose is separated by filtration or centrifugation.

In other words, to extract the precipitated xylose by filtration or centrifugation.

Through this process, pure xylose is extracted.

On the other hand, the last step is to produce xylose through the purification step of purification through the treatment of acid hydrolysis.

In order to increase the purity of xylose is purified through acid hydrolysis treatment.

At this time, sulfuric acid, hydrochloric acid, formic acid, etc. may be used as the acid solution for purification.

The produced xylose is used as a raw material or sweetener of gum.

As described above, the present invention is not the only method of extracting xylose through the steps of concentration, precipitation, filtration and purification in the pre-hydrolysis eluate, and through the step of pre-hydrolysis and cooking. There is also a method of extraction.

Thus, even in this latter case, the following work steps of the first to sixth steps of the above-described contents are similarly followed.

But from the next seventh step, the branch is changed.

That is, in the seventh step, the bamboo chip is administered to the cooking section (Digester), and the ratio of the chemical weight consisting of water, alkali and anthraquinone to the weight of bamboo is 1: 3.5-6.0 (bamboo: chemical solution). It is cooked at high temperature to soften bamboo chips and then pulp.

In other words, when the conventional sulfurous acid method is used for the cooking of the bamboo chips, the fiber is weak and the pulp yield is low.

Therefore, the present invention applies soda-AQ method not only to promote delignification but also to prevent degradation of alpha cellulose and to increase the yield of pulp.

In other words, the soda-AQ method is introduced at a liquid ratio of 3.5-6.0: 1 compared to a liquid containing alkali (mainly NaOH), anthraquinone and water, and a dry bamboo chip.

In addition, the alkali (in terms of Na ₂ O) introduced into the water in the soda-AQ method is 10-30% of totally dry (pure mass excluding moisture contained in bamboo chips) and bamboo anthraquinone (AQ). It is preferable to add 0.01-2%.

In this cooking step, the cooking temperature is 140-180 ° C., and the cooking time is preferably adjusted in accordance with the quality of the pulp to be produced, such as the degree of polymerization, within the range of 90-200 minutes.

Then, the next step is step 8: neutralizing precipitate by supplying carbon dioxide to elute xylose.

In other words, it is used to extract xylose better and to settle and separate xylose.

The next step is step 9: adding water, alcohol, methyl isobutyl ketone mixture and mixing the phases while controlling the proportion of water in a well mixed state.

That is, since the lignin is present in the precipitate after the above step, a phase separation process is required to separate the xylose from the mixture.

That is, lignin is dissolved in an organic solvent, while hemicellulose and xylose are dissolved in an aqueous solution.

Therefore, water, alcohol and methyl isobutyl ketone (methylisobutyl ketone) is added to the mixture for mixing well and then the ratio of water to control the phase separation to occur.

When phase separation occurs, the organic solvent fraction and the aqueous fraction are separated.

In the next step, step 10: adds alcohol to the separated aqueous solution and proceeds to precipitate xylose.

That is, alcohol is distilled off and collected again.

Now look at the embodiment of the present invention with a table shown.

Example 1

Myanmar bamboo was cut into about 2 mm width, cut into 15-25 mm, and then screened using a 60 mesh mesh bucket to remove foreign matter and bamboo debris and then washed.

Take the amount of washed bamboo 400g total amount into the digester, fill the water to adjust the liquid ratio to 6: 1, and then put the stainless steel weight so that the bamboo is sufficiently submerged in water.

The lid of the digester was covered and the screws were tightened, followed by hydrolysis at 170 ° C. for 90 minutes.

After the end of hydrolysis, the separated solution and the water used for washing were concentrated and precipitated by the alkanol method.

The washed prehydrolyzed bamboo chips were added to the digester again, and 16% of activated alkali (in terms of Na ₂ O) and 0.1% of anthraquinone were added, and the liquid ratio was adjusted to 4: 1. Was carried out.

The cooking waste and washings were concentrated and neutralized to precipitate by addition of carbon dioxide.

The precipitate was separated from the alkaline solution, dissolved by addition of a mixture of water, alcohol and methyl isobutyl ketone, and water was added thereto for phase separation. The characteristics of the resulting pulp are shown in Table 1.

Table 1. Experimental results of prehydrolysis and pulping of bamboo 1

Total hydrolysis elution fraction (%) pulp yield (%) aqueous solution in pulp waste (%) kappa 26.3 39.5 15.4 10.5

Example 2

Bamboo treatment and most of the conditions were the same as in Example 1, the conditions of the pre-hydrolysis conditions were applied as follows.

That is, the liquid ratio during prehydrolysis was adjusted to 4: 1, and hydrolysis was performed at 170 ° C. for 100 minutes. The characteristics of the resulting pulp are shown in Table 2.

Table 2. Experimental Results of Prehydrolysis and Pulping of Bamboo 2

Total hydrolysis elution fraction (%) pulp yield (%) aqueous solution in pulp waste (%) kappa 27.6 37.8 13.5 9.8

As described above, the present invention recovers the high value-added resources by recovering xylose generated as a by-product in the process of producing a dissolving pulp using bamboo which can supply a stable raw material without affecting the environment much, thereby making the natural resources more efficient. It is available and recovers xylose at a much lower cost than producing xylose from existing wood or pulp.

In particular, it is possible to selectively apply xylose, which is contained in pre-hydrolysis and xylose contained in the cooking shell, in a separate process, depending on economic feasibility.

The recycling of wastes generated during the dissolution pulp production process helps to improve the economic efficiency, and can bring down the price of xylose used as a manufacturing material for xylitol, sweeteners, and pharmaceuticals.

Claims (6)

delete delete delete delete In the manufacturing method of xylose produced using bamboo, First step: removing bamboo leaves to remove the leaves from the bamboo; Second step: vertical cutting to split the bamboo but cut vertically at intervals of 1.5-3 mm; A third step: a cutting step of producing bamboo chips by cutting horizontally cut bamboo to a length of 10-30 mm; A fourth step: screening to filter debris or impurities from the cut bamboo chips; The fifth step: a washing step of washing impurities, foreign matters and dusts, etc., deposited on the bamboo chips with water; Step 6: Pre-hydrolysis step of washing washed bamboo chips using water or steam for pre-hydrolysis, and adding catalyst to promote pre-hydrolysis according to the required degree of pre-hydrolysis to dissolve hemicellulose Wow; Step 7: The bamboo chip is administered to the cooking section (Digester), and the ratio of the chemical weight consisting of water, alkali, and anthraquinone to the bamboo weight is 1: 3.5-6.0 (bamboo: chemical solution). A cooking step of pulping by softening the bamboo chips by cooking; Eighth step: neutralizing precipitate by supplying carbon dioxide gas to elute xylose; Step 9: adding water, alcohol, methyl isobutyl ketone mixture and phase separation while controlling the proportion of water in a well mixed state; Step 10: Precipitating xylose by adding alcohol to the separated aqueous solution; Xylose production method that is produced using bamboo, characterized in that the production of xylose is made of gum. The method of claim 5, In the seventh step, Alkali (in terms of Na ₂ O) added to water is 10-30% compared to total dry (pure mass except moisture contained in bamboo chips) bamboo chips, and 0.01-2% of anthraquinone (AQ) is added. Method for producing pulp using bamboo characterized in that.