CN1446784A - Method for producing xylitol by using bracteal leaf of maize - Google Patents
Method for producing xylitol by using bracteal leaf of maize Download PDFInfo
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- CN1446784A CN1446784A CN 03111433 CN03111433A CN1446784A CN 1446784 A CN1446784 A CN 1446784A CN 03111433 CN03111433 CN 03111433 CN 03111433 A CN03111433 A CN 03111433A CN 1446784 A CN1446784 A CN 1446784A
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Abstract
A process for preparing xylitol from the bracteal leaf of corn includes hydrolyzing with hydrochloric acid as catalyst to obtain xylose solution, neutralizing with cationic exchange resin, decolouring with activated carbon, and hydrogenating. Its advantage is high quality of product.
Description
Technical Field
The invention relates to a method for producing xylitol, in particular to a method for producing xylitol by using corn bracts.
Background
At present, xylitol (C) is prepared5H12O5) The mature process takes corncobs or bagasse as raw materials, the specific surface area of the corncobs or bagasse is 4cm/g, the corncobs or bagasse is relatively small, the catalysis time is prolonged, and the corncobs or bagasse is subjected to pressurized hydrolysis; the neutralization process employs calcium carbonate (CaCO)3) The neutralizing agent increases ash in the hydrolysate, increases colloid, reduces the quality of the solution, increases burden for next purification, particularly generates serious scale formation during evaporation, influences the normal operation of evaporation, greatly increases the consumption of steam for evaporation, and also generates side effect of the neutralization process, namely an alkali passing area during neutralization, so that the color of the neutralization solution is deepened, and the decomposition and loss of sugar are increased, particularly serious at high temperature and long time; the purification in the process adopts a recrystallization method; due to miningThe corn cob is used as a raw material, the pigment content of the corn cob is obviously greater than that of the corn bracts, the average chroma value of the corn cob is 1.1 Sedengmier, the average chroma value of the corn bracts is 0.6 Sedengmier, and the pigment content of the corn cob is relatively high, so that the consumption of a decoloring agent, namely activated carbon in a decoloring process is large, and the production cost is high; in addition, sulfuric acid (H) is generally used as the catalyst for hydrolysis2SO4) The catalytic activity of sulfuric acid is not very high.
Disclosure of Invention
The invention aims to solve the problems of high cost and poor product quality in the existing xylitol production process, and provides a method for producing xylitol by using corn bracts, which has low production cost, high efficiency and low investment.
The method comprises the following process steps and principles:
(1) pulverizing corn bract, and removing impurities before and after pulverizing;
(2) the crushed corn bracts are subjected to primary water washing, acid washing and secondary water washing, dust impurities in the raw materials can be removed, and the purityof hydrolysate can be relatively improved;
(3) hydrolyzing the treated corn bract to prepare xylose, wherein the technological conditions during hydrolysis are as follows: the temperature is 100-130 ℃, wherein 100-125 is the preferred temperature, and 100-106 is the optimal temperature; the time is 2-3 hours; the catalyst is hydrochloric acid (HCI), the concentration of the hydrochloric acid is 1 percent, the solid-liquid ratio is 1: 10, and the pressure is normal pressure;the principle of hydrolysis is: the corn bract contains pentosan, and the structural formula of the corn bract is as follows:
this can be seen as a polymer formed by dehydration condensation of the hemiacetal group of one pentosan molecule and the hydroxyl group on four carbon atoms of another pentosan molecule, i.e., hemicellulose, which is insoluble in water and has no sweet taste, and is dissolved and further hydrolyzed by heating in an acid aqueous solution, i.e., hydrolyzed into many pentoses, i.e., xylose, of single molecules, according to the following reaction formula:
(4) removing acid in the xylose liquid by using anion exchange resin, wherein the anion exchange resin adopts melamine-guanidine-formaldehyde resin, ammonia water is adopted during regeneration, and regenerated waste liquid contains ammonium chloride for agricultural irrigation;
(5) the activated carbon is utilized to remove pigments and a part of nitrogenous substances in the xylose solution, so that the catalyst poisoning during the subsequent catalytic hydrogenation is avoided; the process conditions in the decoloring procedure are as follows: the temperature is 80 ℃, the heat preservation stirring speed is 37 r/m, the dosage of the active carbon is 10 percent (relative to sugar),and the quality of the decolored liquid is more than 80 percent of the transmittance; the active carbon is a mixture of powder and particles; wherein the powder accounts for 63.6 to 66.7 percent;
(6) evaporating to remove water in the xylose liquid; the process conditions are as follows: the temperature is below 60 ℃, the vacuum degree is above 0.85atm, and the time is 6-9 hours;
(7) purifying and purifying the evaporated xylose by using ion resin, wherein the purity of the evaporated xylose is only about 85 percent generally, and in order to ensure the purity of the xylose for hydrogenation, the xylose for hydrogenation is purified to be more than 95 percent;
the anionic resins used were: melamine resin (AH-1) with exchange capacity of 2.4 milliequivalents/g, specific volume of 2.2-2.8 ml/g and granularity of 0.3-2.0 mm;
the cation resin used is 732#Sulfonic resin (styrene-divinylbenzene strong acid resin), the exchange capacity is 1.1-1.5 milliequivalent/g, and the granularity is 0.25-2.0 mm;
(8) xylose is hydrogenated to prepare xylitol, and the reaction formula is as follows:
the reaction process conditions are as follows: pressure: 6.5-8.0 Mpa, reaction temperature: 110-130 ℃; the catalyst is Raney nickel, and the addition amount of the Raney nickel is 3-6%; the pH value of the solution is 7.5-8, and the reaction time is 60 minutes; the optimal process conditions are as follows: the temperature is 120 ℃, the pressure is 7.5Mpa, the reaction time is 60 minutes, the catalyst dosage is 6 percent, the average conversion rate of xylose is 99.23 percent, and the average yield is 90.59 percent.
The invention has the advantages and positive effects that:
firstly, the content of raw material pigment is low: in China, the traditional xylitol production raw material is mainly corncobs, the average value of the chroma of the corncobs is 1.1 Sedenmil, the average value of the color of the corn bracts is 0.6 Sedenmil, and the pigment content difference between the corncobs and the bracts greatly reduces the consumption of a decoloring agent in a decoloring process, thereby reducing the burden of purification of the subsequent process. At present, the price of the decolorizing agent is higher, and the cost of the decolorizing agent accounts for almost 50 percent of the cost of all raw materials in the production of enterprises. Therefore, the economic benefit of enterprises is obviously improved by taking the corn bracts as the raw materials.
Secondly, influence of temperature and pressure: the method is used for hydrolyzing under the conditions of normal pressure and 100-130 ℃, the traditional production is carried out under pressurization, the color of the xylose solution is increased by 10 times along with the temperature rise, the temperature is not changed, the concentration of acid is increased, the color is increased, but the increase range is small, and the quality of the hydrolysate is good. Therefore, the acid concentration is rather high, and the temperature cannot be high, so that the consumption of the decolorizing agent can be greatly reduced by normal-pressure hydrolysis. In addition, the equipment investment of the pressure hydrolysis is larger than that of the normal pressure hydrolysis equipment.
Influence of specific surface area of raw materials: the specific surface areas of the corncobs and the corn bracts serving as raw materials are greatly different, the specific surface area of the corncobs is 4cm/g, the specific surface area of the corn bracts is 220cm/g, the pretreatment and hydrolysis processes have obvious different effects, thespecific surface area of the corn bracts is large, the corn bracts are easy to hydrolyze thoroughly when acting with a catalyst, the mass and heat transfer effects are obvious, and the catalysis time can be shortened.
Fourthly, although it is believed that hydrochloric acid (HCI) is more likely to be present than sulfuric acid (H)2SO4) The corrosion to equipment is large, but the catalytic activity of hydrochloric acid (HCI) is far greater than that of sulfuric acid (H)2SO4) The concentration of hydrochloric acid (HCI) is sulfuric acid (H) in the amount used2SO4) 1/2 concentration, and both are sold at nearly the same price, so hydrochloric acid (HCI) hydrolysis is economically advantageous.
And fifthly, the neutralization method is different:the conventional neutralization method is CaCO3The method increases ash in the hydrolysate and colloid in the hydrolysate, reduces the quality of the solution, increases the burden of the next purification, particularly generates serious scale during evaporation, influences the normal operation of the evaporation and greatly increases the consumption of steam for evaporation. In addition, the side effect of the neutralization process, i.e. the overbasing zone during neutralization, is produced, which darkens the color of the neutralized liquor and increases the decomposition and loss of sugars, especially at high temperatures and over long periods of time, which the ion exchange method avoids.
Detailed Description
Example 1 of the present invention
(1) Pulverizing corn bract into 1.5 × 0.5cm2And removing impurities in the solution;
(2) taking a proper amount of crushed corn bracts, washing with water, then washing with 1% hydrochloric acid solution, and then washing with water;
(3) feeding the processed corn bracts into a hydrolysis tank for hydrolysis, adding 1% hydrochloric acid, wherein the solid-liquid ratio is 1: 10, the reaction temperature is 100 ℃, and the reaction time is 2.5 hours; the pressure is normal pressure; decomposing into xylose liquid through reaction;
(4) removing acid from the xylose liquor by using melamine-guanidine-formaldehyde resin;
(5) the xylose solution is decolorized by using powdered and granular mixed active carbon, and the process conditions are as follows: the temperature is 80 ℃, the heat preservation stirring speed is 37 r/m, the dosage of the active carbon is 10 percent (relative to sugar), and the quality of the decolored liquid is more than 80 percent of the transmittance;
(6) evaporating to remove water in the xylose liquid; the process conditions are as follows: the temperature is below 60 ℃, the vacuum degree is above 0.85atm, and the time is 6-9 hours;
(7) purifying xylose with melamine resin (AH-1);
(8) xylose is hydrogenated to prepare xylitol, and the reaction process conditions are as follows: the pressure is 6.5Mpa, the reaction temperature is 110 ℃, the catalyst is Raney nickel, the adding amount is 3 percent, and the pH value of the solution is 7.5.
Example 2
Example 1 was repeated with the same procedure as described, except that,
the process conditions of the step (3) are as follows: the temperature is 130 ℃, and the hydrolysis time is 3 hours;
the time in the step (6) is 9 hours;
the resin used in step (7) was 732#Sulfonic acid type (styrene-divinylbenzene strong acid resin);
the process conditions in the step (8) are as follows: the pressure is 8.0Mpa, the reaction temperature is 130 ℃, and the addition amount of the Raney nickel is 5 percent; the pH of the solution was 8.
Example 3
Example 1 was repeated with the same procedure as described, except that,
the technological conditions of the step (3) are that the temperature is 106 ℃, and the hydrolysis time is 2 hours;
the evaporation time in step (6) is 7.5 hours;
the process conditions in the step (8) are as follows: the pressure is 7.5Mpa, the reaction temperature is 120 ℃, the reaction time is 60 minutes, and the adding amount of the Raney nickel is 6 percent;
example 4
Example 3 was repeated with the same procedure as described except that the resin used in step (7) was 732#Sulfonic resin (styrene-divinylbenzene strong acid resin).
In the four examples, the average conversion of xylose was 99.23%, and the average yield was 90.5%.
Claims (10)
1. A method for producing xylitol from corn bracts, which sequentially comprises the following steps:
(1) pulverizing corn bract, and removing impurities before and after pulverizing;
(2) feeding the crushed corn bracts into water, acid and water for treatment;
(3) hydrolyzing the treated corn bract to prepare xylose by using hydrochloric acid as a catalyst;
(4) removing acid in the xylose liquid by using anion exchange resin;
(5) removing pigments and a partof nitrogen-containing substances in the xylose solution by using activated carbon;
(6) evaporating to remove water in the xylose liquid;
(7) purifying and purifying the evaporated xylose by using ion resin;
(8) xylose is hydrogenated to prepare xylitol.
2. The method for producing xylitol according to claim 1, comprising: the hydrolysis process conditions in the step (3) are as follows: the temperature is 100-130 ℃, and the hydrolysis time is 2-3 hours; the concentration of hydrochloric acid is 1%, the solid-liquid ratio is 1: 10, and the pressure is normal pressure.
3. The process for producing xylitol according to claim 2, comprising the steps of: the hydrolysis temperature is 100-106 ℃.
4. The method for producing xylitol according to claim 1, comprising: the melamine-guanidine-formaldehyde resin of the anion exchange resin used in the step (4) adopts ammonia water during regeneration.
5. The method for producing xylitol according to claim 1, comprising: the process conditions in the step (5) are as follows: the temperature is 80 ℃, the heat preservation stirring speed is 37 r/m, the active carbon consumption is 10 percent, and the mass of the decolored liquid is more than 80 percent of the transmittance.
6. The method for producing xylitol according to claim 1, comprising: the process conditions in the step (6) are that the temperature is below 60 ℃, the vacuum degree is above 0.85atm, and the time is 6-9 hours.
7. The methodfor producing xylitol according to claim 1, comprising: what is needed isThe ion resin used in the step (7) is melamine resin or 732#A sulfonic acid type resin.
8. The method for producing xylitol according to claim 1, comprising: the reaction process conditions in the step (8) are as follows: pressure: 6.5-8.0 Mpa, reaction temperature: 110-130 ℃; the catalyst is Raney nickel, and the addition amount of the Raney nickel is 3-6%; the pH value of the solution is 7.5-8, and the reaction time is 60 minutes.
9. The method for producing xylitol according to claim 8, comprising: the optimal process conditions of the reaction are as follows: the temperature is 120 ℃, the pressure is 7.5Mpa, the reaction time is 60 minutes, and the adding amount of the Raney nickel is 6 percent.
10. The method for producing xylitol according to claim 1, comprising: the active carbon is a mixture of granules and particles, wherein the powder accounts for 63.6-66.7%.
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| CN 03111433 CN1446784A (en) | 2003-04-10 | 2003-04-10 | Method for producing xylitol by using bracteal leaf of maize |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1319980C (en) * | 2005-07-12 | 2007-06-06 | 尤新 | Process for preparing crystalline xylose by hydrolysis of maize peel |
| CN102976895A (en) * | 2012-12-12 | 2013-03-20 | 郑州金土地能源科技有限公司 | Method for producing xylitol through utilizing crop wastes |
| CN103695571A (en) * | 2013-12-16 | 2014-04-02 | 长春工业大学 | Method for preparing xylose and hydrolyzed protein by treating distiller's grains by utilizing subcritical water |
| US10759727B2 (en) | 2016-02-19 | 2020-09-01 | Intercontinental Great Brands Llc | Processes to create multiple value streams from biomass sources |
-
2003
- 2003-04-10 CN CN 03111433 patent/CN1446784A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1319980C (en) * | 2005-07-12 | 2007-06-06 | 尤新 | Process for preparing crystalline xylose by hydrolysis of maize peel |
| CN102976895A (en) * | 2012-12-12 | 2013-03-20 | 郑州金土地能源科技有限公司 | Method for producing xylitol through utilizing crop wastes |
| CN102976895B (en) * | 2012-12-12 | 2015-09-30 | 郑州金土地能源科技有限公司 | Wastes of crops is utilized to make the method for Xylitol |
| CN103695571A (en) * | 2013-12-16 | 2014-04-02 | 长春工业大学 | Method for preparing xylose and hydrolyzed protein by treating distiller's grains by utilizing subcritical water |
| CN103695571B (en) * | 2013-12-16 | 2015-08-05 | 长春工业大学 | Subcritical water process vinasse are utilized to prepare the method for wood sugar and protolysate |
| US10759727B2 (en) | 2016-02-19 | 2020-09-01 | Intercontinental Great Brands Llc | Processes to create multiple value streams from biomass sources |
| US11840500B2 (en) | 2016-02-19 | 2023-12-12 | Intercontinental Great Brands Llc | Processes to create multiple value streams from biomass sources |
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