CN102838451A - Method of preparing xylitol by utilizing of corncob - Google Patents

Method of preparing xylitol by utilizing of corncob Download PDF

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Publication number
CN102838451A
CN102838451A CN 201210305845 CN201210305845A CN102838451A CN 102838451 A CN102838451 A CN 102838451A CN 201210305845 CN201210305845 CN 201210305845 CN 201210305845 A CN201210305845 A CN 201210305845A CN 102838451 A CN102838451 A CN 102838451A
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Prior art keywords
xylitol
exchange resin
corn cob
resin columns
utilizing
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CN 201210305845
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Chinese (zh)
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周冬霞
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Individual
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Individual
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Abstract

The invention relates to a production method of functional sugar, in particular to a method of preparing xylitol by utilizing of corncobs. The method of preparing the xylitol by utilizing of the corncobs is simple in process, low in cost, little in investment and simple in equipment. The method of preparing the xylitol by utilizing of the corncobs includes eight procedures including raw material selection and preparation, acidic hydrolysis, neutralizing treatment, decoloration and evaporation, ion exchange, hydrogenation reaction, concentrate crystal separation, and drying and package. In the procedure of the ion exchange, 732 cation exchange resin columns are in serial connection with porous anion exchange resin columns to purify the xylitol. Concentrated solutions after decoloration and evaporation, from top to bottom, enter the 732 cation exchange resin columns, and then enter the porous anion exchange resin columns, so colorless transparent xylitol liquid is achieved. Ash and cations are eliminated through the 732 cation exchange resin columns, and meanwhile colloids and non sugar bodies are eliminated in an adsorption mode. Residual vitriol anions are eliminated through the porous anion exchange resin columns, purity of the xylitol is improved, equipment scaling is reduced, and product quality is improved.

Description

Utilize corn cob to prepare the method for Xylitol
Technical field
The present invention relates to a kind of working method of functional sugar, be specially a kind of method of utilizing corn cob to prepare Xylitol.
Background technology
Xylitol (C 5H 12O 5), have another name called pentitol, be a kind of five-carbon sugar alcohol.Xylitol is the intermediate product of xylose metabolism, and profile is the crystallinity white powder, and water absorbability is arranged, and nontoxic free from extraneous odour is pleasantly sweet, and is very easily water-soluble, is slightly soluble in ethanol and methyl alcohol.Extensively be present in the plant such as group food and timber, straw, corn cob of fruit, vegetables, cereal, mushroom.Xylitol can be used as the widespread use in industry such as chemical industry, food, medicine of sweeting agent, nutrition agent and medicament.
Xylitol can be participated in body metabolism as a kind of functional sweetener, get into blood after, do not need Regular Insulin just can penetrate cell and accretion rate is fast, can not cause blood sugar increasing, be best suited for nutritional type sugar substitute in patients with diabetes mellitus.Xylitol also has special biochemical property except that the general character with sucrose, glucose, it need not pass through Regular Insulin, just can see through cell walls and be absorbed by the body, and functions such as reduce fat, anti-ketoboidies are arranged.Xylitol is a kind of sweet taste substance with nutritive value, also is the normal midbody of human body sugar metabolism.The people of a health even do not eat any food that contains Xylitol, is also contained the Xylitol of 0.03-0.06 milligram in per 100 milligrams blood.At occurring in nature, Xylitol extensively is present in various fruit, the vegetables, but content is very low.The commodity Xylitol is with in the agricultural crops such as corn cob, bagasse, makes through deep processing, and be a kind of sweeting agent of natural health.The Xylitol white crystal, appearance is similar with sucrose, is sweeting agent the sweetest in the polyvalent alcohol, and flavor is cool, sugariness is equivalent to sucrose, and heat is equivalent to glucose, is following sweeting agent, is sucrose and glucose substitute.
Simultaneously, the prevention of dental caries characteristic of Xylitol effect in all sweeting agents is best, at first is Xylitol can not be produced carious tooth in the oral cavity fermentation using bacteria utilization, suppresses the generation of streptococcus growth and acid; Secondly when chewing Xylitol, can promote salivation, saliva is many both can wash the bacterium in oral cavity, the tooth; Also can increase saliva and carious tooth spot place's basic aminoacids and ammonia concentration, slow down pH value decline in the oral cavity simultaneously, the acidic substance of injury tooth are neutralized dilution; Suppressed the absorption of bacterium at dental surface; Thereby reduced the acid etching of tooth, prevented carious tooth and the generation that reduces dental plaque, consolidated tooth.Xylitol is unique polyol, and it can forbid individually that the streptococcus mutant xenogeneic increases, thereby alleviates the infection rate of carious tooth.Xylitol can be by decayed tooth bacterium fermentation and acid corrosion tooth, and the pure and fresh sweet taste of Xylitol can also promote the secretion of saliva simultaneously, replenishes phosphorus and calcium in the saliva, promotes repairing naturally of tooth.
Xylitol is compared with common white sugar; Have the low advantage of heat, every gram Xylitol only contains 2.4 caloric heats, than the less calories 40% of other most of glucide; Thereby Xylitol can be applied in the various diet food, as the surrogate of high calorie white sugar.But on the technology of producing Xylitol, there are a lot of problems now; As there are differences aspect the selection of raw material; The Xylitol quality that causes producing differs; Because of Xylitol is increasing as the industrial raw material demand over the years, need seek a perfect standard and quality again so produce the raw material of Xylitol.Secondly, be exactly in process of production, complex process, equipment cost is high, and is wayward, thereby reduced yield of product and the recovery and purity.
Summary of the invention
In order to overcome the problem that in producing the Xylitol production process, produces, the object of the invention just is to provide a kind of technology simple, and cost is low, less investment, and equipment simply utilizes corn cob to prepare the method for Xylitol.
The present invention utilizes corn cob to prepare the method for Xylitol, comprises that the raw material choosing is equipped with, acidic hydrolysis, neutralizing treatment, decolouring evaporation, IX, hydrogenation reaction, condensing crystal separates and eight steps of dry packing play; It is characterized in that the described IX step adopts the series connection of 732 type cation exchange resin columns and Decolorite post that Xylitol is purified in playing; Make the liquid concentrator after decolouring is evaporated be introduced into 732 type cation exchange resin columns from top to bottom, get into the Decolorite post again, obtain water white wood sugar liquid.
Further, described condensing crystal separates during the step plays, and comprises that also the step that mother liquor reclaims plays, and mother liquor is earlier through purifying treatment, again through condensing crystal, can access purity and be not less than 90% Xylitol.
Further, the choosing of described raw material is equipped with during the step plays, and selects the white corn cob of water cut at 10%-15%, pulverizes the back and crosses 10 mesh sieves, and doubly moved in the pre-treatment still insulation 1-2 hour to the ionized water of quality with 3-5, and is air-dry behind the filter residue, for use.
Further, in the described acidic hydrolysis, adopt the low-pressure water solution, wherein sulfuric acid concentration is 0.5%-1.5%, and the pH value is 0.8-1.2, and hydrolysis temperature is 110-130 ℃, hydrolysis time 3-5 hour.
Further, the described neutralizing treatment step adopts calcium carbonate emulsion to neutralize in playing; When heating to 75-80 ℃ then, stir on the limit, and the limit adds the calcium carbonate emulsion of Baume 15 degree; Is the point of neutralization up to the pH value for 2.3-3.0, and insulation growing the grain 1 hour is through pressure filter filtering calcium sulfate slag.
Further, during described hydrogenation reaction went on foot and plays, hydrogenation pressure was 70-80kg/cm 2Between, temperature is 110-120 ℃, is 0.8-1 with respect to the charging speed ratio of catalyst volume.
Further, described condensing crystal separates during the step plays, and carries out evaporation concentration in two steps, and the first step is the 700mm mercury column in vacuum tightness, and temperature is under 50 ℃ the situation, is concentrated to contain alcohol 50%; Second step was adopted lift-film evaporator, and vacuum tightness is brought up to more than the 700mm mercury column, and temperature is brought up to 70-75 ℃, was concentrated to contain alcohol and get final product discharging greater than 90%, was pressed into crystallizer, carried out crystallization.
The present invention utilizes corn cob to prepare the method for Xylitol, through adopting 732 type cation exchange resin columns to removing ash and positively charged ion, can also remove colloid and non-sugared body with the form of absorption simultaneously; Utilize Decolorite to the residual sulfuric acid negatively charged ion, and can also adsorb colloidal impurity and the pigment of removing part, improved the purity of Xylitol, reduced equipment scaling; Improved the quality of product greatly, and reclaimed output and the utilization ratio of raw materials improved product, cooperated the meticulous control that each step plays again, simplified technology through mother liquor; Made things convenient for production, its beneficial effect is that reasonable in design, technology is simple; Input cost is low, and product quality is high, and equipment loss is little; Output is high, and energy consumption is low, is suitable for promoting.
Embodiment
Instance 1
The present invention utilizes corn cob to prepare the method for Xylitol, comprises that the following step plays:
1) raw material selects the alternative water cut at 10% white corn cob, pulverizes the back and crosses 10 mesh sieves, and moved in the pre-treatment still insulation 1 hour with 3 times of ionized waters to quality, and is air-dry behind the filter residue, for use.
2) acidic hydrolysis adopts the low-pressure water solution, and wherein sulfuric acid concentration is 0.5%, and the pH value is 0.8, and hydrolysis temperature is 110 ℃, hydrolysis time 3 hours.
3) neutralizing treatment adopts calcium carbonate emulsion to neutralize, and when heating to 75 ℃ then, stir on the limit, and the limit adds the calcium carbonate emulsion of Baume 15 degree, is 2.3 to be the point of neutralization up to pH value, is incubated growing the grain 1 hour, through pressure filter filtering calcium sulfate slag.
4) decolouring evaporation.
5) IX adopts the series connection of 732 type cation exchange resin columns and Decolorite post that Xylitol is purified; Make the liquid concentrator after decolouring is evaporated be introduced into 732 type cation exchange resin columns from top to bottom, get into the Decolorite post again, obtain water white wood sugar liquid.
6) hydrogenation reaction, hydrogenation pressure are 70kg/cm 2Between, temperature is 110-120 ℃, is 0.8 with respect to the charging speed ratio of catalyst volume.
7) condensing crystal separates, and carries out evaporation concentration in two steps, and the first step is the 700mm mercury column in vacuum tightness, and temperature is under 50 ℃ the situation, is concentrated to contain alcohol 50%; Second step was adopted lift-film evaporator, and vacuum tightness is brought up to more than the 700mm mercury column, and temperature is brought up to 70 ℃, was concentrated to contain alcohol and get final product discharging greater than 90%, was pressed into crystallizer, carried out crystallization.Comprise also that wherein the step that mother liquor reclaims plays, mother liquor is earlier through purifying treatment, again through condensing crystal, can access purity and be not less than 90% Xylitol.
8) dry packing.
Instance 2
The present invention utilizes corn cob to prepare the method for Xylitol, comprises that the following step plays:
1) raw material selects the alternative water cut at 12% white corn cob, pulverizes the back and crosses 10 mesh sieves, and doubly moved in the pre-treatment still insulation 1.5 hours to the ionized water of quality with 3-5, and is air-dry behind the filter residue, for use.
2) acidic hydrolysis adopts the low-pressure water solution, and wherein sulfuric acid concentration is 1%, and the pH value is 1, and hydrolysis temperature is 120 ℃, hydrolysis time 4 hours.
3) neutralizing treatment adopts calcium carbonate emulsion to neutralize, and when heating to 78 ℃ then, stir on the limit, and the limit adds the calcium carbonate emulsion of Baume 15 degree, is 2.5 to be the point of neutralization up to pH value, is incubated growing the grain 1 hour, through pressure filter filtering calcium sulfate slag.
4) decolouring evaporation.
5) IX adopts the series connection of 732 type cation exchange resin columns and Decolorite post that Xylitol is purified; Make the liquid concentrator after decolouring is evaporated be introduced into 732 type cation exchange resin columns from top to bottom, get into the Decolorite post again, obtain water white wood sugar liquid.
6) hydrogenation reaction, hydrogenation pressure are 75kg/cm 2Between, temperature is 115 ℃, is 09 with respect to the charging speed ratio of catalyst volume.
7) condensing crystal separates, and carries out evaporation concentration in two steps, and the first step is the 700mm mercury column in vacuum tightness, and temperature is under 50 ℃ the situation, is concentrated to contain alcohol 50%; Second step was adopted lift-film evaporator, and vacuum tightness is brought up to more than the 700mm mercury column, and temperature is brought up to 72 ℃, was concentrated to contain alcohol and get final product discharging greater than 90%, was pressed into crystallizer, carried out crystallization.Comprise also that wherein the step that mother liquor reclaims plays, mother liquor is earlier through purifying treatment, again through condensing crystal, can access purity and be not less than 90% Xylitol.
8) dry packing.
Instance 3
The present invention utilizes corn cob to prepare the method for Xylitol, comprises that the following step plays:
1) raw material selects the alternative water cut at 15% white corn cob, pulverizes the back and crosses 10 mesh sieves, and moved in the pre-treatment still insulation 2 hours with 5 times of ionized waters to quality, and is air-dry behind the filter residue, for use.
2) acidic hydrolysis adopts the low-pressure water solution, and wherein sulfuric acid concentration is 1.5%, and the pH value is 1.2, and hydrolysis temperature is 130 ℃, hydrolysis time 5 hours.
3) neutralizing treatment adopts calcium carbonate emulsion to neutralize, and when heating to 80 ℃ then, stir on the limit, and the limit adds the calcium carbonate emulsion of Baume 15 degree, is 3.0 to be the point of neutralization up to pH value, is incubated growing the grain 1 hour, through pressure filter filtering calcium sulfate slag.
4) decolouring evaporation.
5) IX adopts the series connection of 732 type cation exchange resin columns and Decolorite post that Xylitol is purified; Make the liquid concentrator after decolouring is evaporated be introduced into 732 type cation exchange resin columns from top to bottom, get into the Decolorite post again, obtain water white wood sugar liquid.
6) hydrogenation reaction, hydrogenation pressure are 80kg/cm 2Between, temperature is 120 ℃, is 1 with respect to the charging speed ratio of catalyst volume.
7) condensing crystal separates, and carries out evaporation concentration in two steps, and the first step is the 700mm mercury column in vacuum tightness, and temperature is under 50 ℃ the situation, is concentrated to contain alcohol 50%; Second step was adopted lift-film evaporator, and vacuum tightness is brought up to more than the 700mm mercury column, and temperature is brought up to 75 ℃, was concentrated to contain alcohol and get final product discharging greater than 90%, was pressed into crystallizer, carried out crystallization.Comprise also that wherein the step that mother liquor reclaims plays, mother liquor is earlier through purifying treatment, again through condensing crystal, can access purity and be not less than 90% Xylitol.
8) dry packing.

Claims (7)

1. utilize corn cob to prepare the method for Xylitol, comprise that the raw material choosing is equipped with, acidic hydrolysis, neutralizing treatment, decolouring evaporation, IX, hydrogenation reaction, condensing crystal separates and eight steps of dry packing play; It is characterized in that the described IX step adopts the series connection of 732 type cation exchange resin columns and Decolorite post that Xylitol is purified in playing; Make the liquid concentrator after decolouring is evaporated be introduced into 732 type cation exchange resin columns from top to bottom, get into the Decolorite post again, obtain water white wood sugar liquid.
2. the method for utilizing corn cob to prepare Xylitol according to claim 1 is characterized in that, during described condensing crystal separation goes on foot and plays; The step that also comprises the mother liquor recovery plays; Mother liquor is earlier through purifying treatment, again through condensing crystal, can access purity and be not less than 90% Xylitol.
3. the method for utilizing corn cob to prepare Xylitol according to claim 1 and 2; It is characterized in that described raw material choosing is selected the white corn cob of water cut at 10%-15% in going on foot fully and playing; Pulverize the back and cross 10 mesh sieves; And doubly moved in the pre-treatment still insulation 1-2 hour to the ionized water of quality with 3-5, air-dry behind the filter residue, for use.
4. the method for utilizing corn cob to prepare Xylitol according to claim 1 and 2 is characterized in that, in the described acidic hydrolysis; Adopt the low-pressure water solution, wherein sulfuric acid concentration is 0.5%-1.5%, and the pH value is 0.8-1.2; Hydrolysis temperature is 110-130 ℃, hydrolysis time 3-5 hour.
5. the method for utilizing corn cob to prepare Xylitol according to claim 1 and 2 is characterized in that, during described neutralizing treatment goes on foot and plays; Adopt calcium carbonate emulsion to neutralize, when heating to 75-80 ℃ then, stir on the limit; The limit adds the calcium carbonate emulsion of Baume 15 degree; Is the point of neutralization up to the pH value for 2.3-3.0, and insulation growing the grain 1 hour is through pressure filter filtering calcium sulfate slag.
6. the method for utilizing corn cob to prepare Xylitol according to claim 1 and 2 is characterized in that, during described hydrogenation reaction went on foot and plays, hydrogenation pressure was 70-80kg/cm 2Between, temperature is 110-120 ℃, is 0.8-1 with respect to the charging speed ratio of catalyst volume.
7. the method for utilizing corn cob to prepare Xylitol according to claim 1 and 2 is characterized in that, during described condensing crystal separation goes on foot and plays; Carry out evaporation concentration in two steps; The first step is the 700mm mercury column in vacuum tightness, and temperature is under 50 ℃ the situation, is concentrated to contain alcohol 50%; Second step was adopted lift-film evaporator, and vacuum tightness is brought up to more than the 700mm mercury column, and temperature is brought up to 70-75 ℃, was concentrated to contain alcohol and get final product discharging greater than 90%, was pressed into crystallizer, carried out crystallization.
CN 201210305845 2012-08-23 2012-08-23 Method of preparing xylitol by utilizing of corncob Pending CN102838451A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104762333A (en) * 2015-03-09 2015-07-08 浙江工业大学 A method of preparing xylitol by utilization of winter bamboo shoot shells
CN105622339A (en) * 2016-04-01 2016-06-01 张喜强 Xylitol extraction process
CN107602344A (en) * 2017-08-10 2018-01-19 合肥果成科技有限公司 A kind of Xylitol production technology
CN111567800A (en) * 2020-05-26 2020-08-25 江苏周春祥生物科技有限公司 Sweet composition capable of replacing sucrose and preparation method thereof
US10759727B2 (en) 2016-02-19 2020-09-01 Intercontinental Great Brands Llc Processes to create multiple value streams from biomass sources

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104762333A (en) * 2015-03-09 2015-07-08 浙江工业大学 A method of preparing xylitol by utilization of winter bamboo shoot shells
CN104762333B (en) * 2015-03-09 2018-05-22 浙江工业大学 The method that xylitol is prepared using winter bamboo shoot shell
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
CN105622339A (en) * 2016-04-01 2016-06-01 张喜强 Xylitol extraction process
CN107602344A (en) * 2017-08-10 2018-01-19 合肥果成科技有限公司 A kind of Xylitol production technology
CN111567800A (en) * 2020-05-26 2020-08-25 江苏周春祥生物科技有限公司 Sweet composition capable of replacing sucrose and preparation method thereof

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Application publication date: 20121226