CN113897464A - Control method for refining high-granularity process of semi-fiber xylose - Google Patents
Control method for refining high-granularity process of semi-fiber xylose Download PDFInfo
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- CN113897464A CN113897464A CN202111026611.XA CN202111026611A CN113897464A CN 113897464 A CN113897464 A CN 113897464A CN 202111026611 A CN202111026611 A CN 202111026611A CN 113897464 A CN113897464 A CN 113897464A
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- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
- C13K13/00—Sugars not otherwise provided for in this class
- C13K13/002—Xylose
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Abstract
The invention relates to the technical field of xylose production, in particular to a high-granularity process control method for refining xylose by semi-fiber, which comprises the following steps: hemicellulose extraction, hemicellulose acid hydrolysis, decoloration treatment, electrodialysis treatment, ion exchange treatment, evaporation concentration, cooling crystallization, centrifugation treatment, drying treatment and xylose packaging; the evaporation concentration specifically refers to controlling the purity and refraction of xylose by evaporation concentration, controlling the refraction of xylose with the purity of 75-78% to be 78-79%, or controlling the refraction of xylose with the purity of 72-75% to be 79-80%; the cooling crystallization specifically comprises the following steps: optimizing the reduction rate of the initial crystal grain generation temperature of the xylose crystal by optimizing the temperature, cooling by adopting 0.25-0.35 ℃ per hour when the temperature is reduced to 55 ℃, and cooling by adopting a rapid cooling mode at 55-32 ℃. By the control method, the grain diameter proportion of more than 80 meshes can be effectively increased, and the problem that the granularity of a finished product cannot meet the requirement is effectively solved.
Description
Technical Field
The invention relates to the technical field of xylose production, in particular to a high-granularity process control method for refining xylose from semi-fiber.
Background
At present, the international xylose market is competitively excited, the market is opened by needing good product quality, the requirement on xylose particles is more than 80 meshes internationally, and if most of the particles in the current xylose process are improved to more than 80 meshes, the finished product delivery quality is improved to a great extent, the customer acceptance degree is improved, and the finished product can smoothly enter the export refined xylose market.
At present, 407 batches of finished products of the first three xylose plants in the national yield are detected together, wherein 14 batches of the finished products with the grain diameter of more than 80 meshes accounting for more than 20 percent are totally detected, and 2 batches of the finished products with the grain diameter of more than 80 meshes accounting for more than 30 percent are totally detected, so that the export requirement cannot be met.
Disclosure of Invention
In order to solve the technical problems, the invention provides a semi-fiber xylose refining high-granularity process control method, which can effectively solve the problem that the granularity of a finished product cannot meet the requirement by effectively accounting for the particle size of more than 80 meshes.
The invention is realized by adopting the following technical scheme:
a semi-fiber xylose refining high-granularity process control method is characterized by comprising the following steps: the method comprises the following steps: hemicellulose extraction, hemicellulose acid hydrolysis, decoloration treatment, electrodialysis treatment, ion exchange treatment, evaporation concentration, cooling crystallization, centrifugation treatment, drying treatment and xylose packaging; the evaporation concentration specifically refers to controlling the purity and refraction of xylose by evaporation concentration, controlling the refraction of xylose with the purity of 75-78% to be 78-79%, or controlling the refraction of xylose with the purity of 72-75% to be 79-80%; the cooling crystallization specifically comprises the following steps: optimizing the reduction rate of the initial crystal grain generation temperature of the xylose crystal by optimizing the temperature, cooling by adopting 0.25-0.35 ℃ per hour when the temperature is reduced to 55 ℃, and cooling by adopting a rapid cooling mode at 55-32 ℃.
The centrifugal treatment specifically refers to centrifugation by adopting an upper spin type centrifuge or a three-leg type centrifuge.
During the evaporation concentration, the purity of xylose during the evaporation concentration is controlled by recovering xylose with 99 percent of purity.
In the process of evaporation concentration, the final refraction of evaporation concentration is controlled by spraying water mist.
During the evaporation concentration process, the refraction fluctuation is controlled to be +/-0.1 by spraying water mist.
In the cooling crystallization process, cooling water with lower temperature is used to realize rapid cooling.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, through two treatment steps of evaporation concentration and cooling crystallization, key factors influencing the particle size of the xylose finished product are controlled, and through the control of concentration, refraction and temperature, the particle size is controlled, and the particle size ratio of more than 80 meshes is effectively increased. In the invention, the xylose with the purity of 75-78 percent is controlled to reflect 78-79 percent of light, or the xylose with the purity of 72-75 percent reflects 79-80 percent of light, the purity and the crystallization can reach the maximum yield under the corresponding relation, and the crystallization can be avoided from being generated before entering the crystallization tank. In the crystal generation stage, when the temperature is reduced to 55 ℃ at 70 ℃, the temperature is reduced by 0.25-0.35 ℃ per hour, and the phenomenon that a large number of crystal nuclei are generated due to too fast temperature reduction is avoided, so that the final crystal particles are reduced, and in the crystal nucleus forming stage, the temperature is slower, and the forming probability of large-particle crystals can be effectively improved.
2. In the invention, the centrifugal treatment specifically refers to centrifugation by adopting an upper spin type centrifuge or a three-foot type centrifuge, the two centrifuges have obvious effect of improving the particle size of 20-80 meshes, and the percentage of particles of 20-80 meshes is improved by 5-6 percentage points compared with that of a lower spin type centrifuge.
3. The purity of xylose during evaporation concentration is controlled by blending xylose with 99 percent purity, the separation liquid is fully utilized, resources are saved, and the purity control effect is good.
4. In the evaporation concentration process, the final refraction of evaporation concentration is controlled by water mist spraying, because the evaporation refraction of the xylose is not easy to be accurate, the refraction fluctuation is +/-0.5, the raw material can be excessively evaporated by water mist spraying, and then the refraction fluctuation is +/-0.1 by water mist spraying and accurate control.
Drawings
The invention will be described in further detail with reference to the following description taken in conjunction with the accompanying drawings and detailed description, in which:
FIG. 1 is a schematic flow chart of the present invention.
Detailed Description
Example 1
The invention discloses a high-granularity process control method for refining xylose from semi-fiber, which comprises the following steps: hemicellulose extraction, hemicellulose acid hydrolysis, decoloration treatment, electrodialysis treatment, ion exchange treatment, evaporation concentration, cooling crystallization, centrifugation treatment, drying treatment and xylose packaging. Wherein the hemicellulose extraction comprises obtaining the wood pulp by utilizing the felling residues, the wood-making residues and the processing residues, soaking in alkali liquor to extract cellulose to obtain alkali-containing liquid hemicellulose, and then carrying out dealkalization treatment.
In the evaporation concentration stage, the purity of xylose in evaporation concentration is controlled by returning xylose with 99% purity to ensure that the purity is 75%, the final refraction of evaporation concentration is controlled by spraying water mist, the refraction is controlled to be 79%, and the fluctuation of the refraction is controlled to be +/-0.1. And in the process of cooling crystallization, cooling water with lower temperature is used, so that rapid cooling is realized. When the temperature is reduced to 55 ℃ from 70 ℃, the temperature is reduced by adopting 0.25 ℃ per hour, and the temperature is reduced by adopting a rapid cooling mode at 55-32 ℃. In the centrifugal treatment stage, an upper spin type centrifuge is used for centrifugation.
Example 2
The rest steps are the same as the step 1, and in the evaporation concentration stage, the purity is controlled to be 78 percent, and the refraction is controlled to be 78 percent. And (3) cooling crystallization, wherein when the temperature is reduced to 55 ℃ at 70 ℃, the temperature is reduced by adopting 0.35 ℃ per hour, and the temperature is reduced by adopting a rapid cooling mode at 55-32 ℃. In the centrifugal treatment stage, an upper spin type centrifuge is used for centrifugation.
Example 3
The rest steps are the same as the step 1, and in the evaporation concentration stage, the purity is controlled to be 72 percent, and the refraction is controlled to be 80 percent. And (3) cooling crystallization, wherein when the temperature is reduced to 55 ℃ at 70 ℃, the temperature is reduced by adopting 0.3 ℃ per hour, and the temperature is reduced by adopting a rapid cooling mode at 55-32 ℃. In the centrifugal treatment stage, an upper spin type centrifuge is used for centrifugation.
Example 4
The rest steps are the same as the step 1, and in the evaporation concentration stage, the purity is controlled to be 74 percent, and the refraction is controlled to be 79.5 percent. And (3) cooling crystallization, wherein when the temperature is reduced to 55 ℃ at 70 ℃, the temperature is reduced by adopting 0.28 ℃ per hour, and the temperature is reduced by adopting a rapid cooling mode at 55-32 ℃. In the centrifugal treatment stage, a three-leg centrifuge is used for centrifugation.
Example 5
The rest steps are the same as the step 1, and in the evaporation concentration stage, the purity is controlled to be 76 percent, and the refraction is controlled to be 78.5 percent. And (3) cooling crystallization, wherein when the temperature is reduced to 55 ℃ from 70 ℃, cooling is carried out at 0.32 ℃ per hour, and cooling is carried out at 55-32 ℃ in a rapid cooling mode. In the centrifugal treatment stage, a three-leg centrifuge is used for centrifugation.
Example 6
The rest steps are the same as the step 1, and in the evaporation concentration stage, the purity is controlled to be 73 percent, and the refraction is controlled to be 79.2 percent. And (3) cooling crystallization, wherein when the temperature is reduced to 55 ℃ at 70 ℃, the temperature is reduced by adopting 0.28 ℃ per hour, and the temperature is reduced by adopting a rapid cooling mode at 55-32 ℃. In the centrifugal treatment stage, a three-leg centrifuge is used for centrifugation.
The data obtained for each example are shown in the following table:
the experiment shows that the particle size ratio of more than 80 meshes can be effectively improved by controlling the concentration, refraction and temperature.
In summary, after reading the present disclosure, those skilled in the art should make various other modifications without creative efforts according to the technical solutions and concepts of the present disclosure, which are within the protection scope of the present disclosure.
Claims (6)
1. A semi-fiber xylose refining high-granularity process control method is characterized by comprising the following steps: the method comprises the following steps: hemicellulose extraction, hemicellulose acid hydrolysis, decoloration treatment, electrodialysis treatment, ion exchange treatment, evaporation concentration, cooling crystallization, centrifugation treatment, drying treatment and xylose packaging; the evaporation concentration specifically refers to controlling the purity and refraction of xylose by evaporation concentration, controlling the refraction of xylose with the purity of 75-78% to be 78-79%, or controlling the refraction of xylose with the purity of 72-75% to be 79-80%; the cooling crystallization specifically comprises the following steps: optimizing the reduction rate of the initial crystal grain generation temperature of the xylose crystal by optimizing the temperature, cooling by adopting 0.25-0.35 ℃ per hour when the temperature is reduced to 55 ℃, and cooling by adopting a rapid cooling mode at 55-32 ℃.
2. The method for controlling the refining high-granularity process of the xylose prepared from the hemicellulose according to the claim 1 is characterized in that: the centrifugal treatment specifically refers to centrifugation by adopting an upper spin type centrifuge or a three-leg type centrifuge.
3. The method for controlling the refining high-granularity process of the xylose prepared from the hemicellulose according to the claim 1 is characterized in that: during the evaporation concentration, the purity of xylose during the evaporation concentration is controlled by recovering xylose with 99 percent of purity.
4. The method for controlling the refining high-granularity process of the xylose prepared from the hemicellulose according to the claim 3 is characterized in that: in the process of evaporation concentration, the final refraction of evaporation concentration is controlled by spraying water mist.
5. The method for controlling the refining high-granularity process of the xylose prepared from the hemicellulose according to the claim 4 is characterized in that: during the evaporation concentration process, the refraction fluctuation is controlled to be +/-0.1 by spraying water mist.
6. The method for controlling the refining high-granularity process of the xylose prepared from the hemicellulose according to the claim 1 is characterized in that: in the cooling crystallization process, cooling water with lower temperature is used to realize rapid cooling.
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| CN202111026611.XA CN113897464A (en) | 2021-09-02 | 2021-09-02 | Control method for refining high-granularity process of semi-fiber xylose |
| CN202210645735.4A CN115044713A (en) | 2021-09-02 | 2022-06-08 | Control method of semi-fiber xylose refining high-granularity process |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115044713A (en) * | 2021-09-02 | 2022-09-13 | 四川雅华生物有限公司 | Control method of semi-fiber xylose refining high-granularity process |
| CN116063158A (en) * | 2022-12-17 | 2023-05-05 | 浙江华康药业股份有限公司 | Induction nucleation crystallization method for improving anti-caking performance of xylitol |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004074519A1 (en) * | 1995-03-01 | 2004-09-02 | Mirja Lindroos | Method for recovery of xylose from solutions |
| CN1805969A (en) * | 2003-06-10 | 2006-07-19 | 格泰克瓜纳巴拉化学工业股份有限公司 | Process for the production of crystalline xylose from sugar cane bagasse, crystalline xylose obtained by said process, process for the production of xylitol from the said xylose and crystalline xylito |
| CN105713998A (en) * | 2016-05-09 | 2016-06-29 | 哈尔滨友利木糖醇科技有限公司 | Production technique of xylose |
| CN109517860A (en) * | 2018-12-07 | 2019-03-26 | 浙江华康药业股份有限公司 | A method of crystal xylose is prepared using xylose mother liquid |
| CN113248551A (en) * | 2021-05-25 | 2021-08-13 | 浙江华康药业股份有限公司 | System and method for preparing refined xylose by utilizing xylose mother liquor chromatographic extract |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113897464A (en) * | 2021-09-02 | 2022-01-07 | 四川雅华生物有限公司 | Control method for refining high-granularity process of semi-fiber xylose |
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- 2021-09-02 CN CN202111026611.XA patent/CN113897464A/en active Pending
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- 2022-06-08 CN CN202210645735.4A patent/CN115044713A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004074519A1 (en) * | 1995-03-01 | 2004-09-02 | Mirja Lindroos | Method for recovery of xylose from solutions |
| CN1805969A (en) * | 2003-06-10 | 2006-07-19 | 格泰克瓜纳巴拉化学工业股份有限公司 | Process for the production of crystalline xylose from sugar cane bagasse, crystalline xylose obtained by said process, process for the production of xylitol from the said xylose and crystalline xylito |
| CN105713998A (en) * | 2016-05-09 | 2016-06-29 | 哈尔滨友利木糖醇科技有限公司 | Production technique of xylose |
| CN109517860A (en) * | 2018-12-07 | 2019-03-26 | 浙江华康药业股份有限公司 | A method of crystal xylose is prepared using xylose mother liquid |
| CN113248551A (en) * | 2021-05-25 | 2021-08-13 | 浙江华康药业股份有限公司 | System and method for preparing refined xylose by utilizing xylose mother liquor chromatographic extract |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115044713A (en) * | 2021-09-02 | 2022-09-13 | 四川雅华生物有限公司 | Control method of semi-fiber xylose refining high-granularity process |
| CN116063158A (en) * | 2022-12-17 | 2023-05-05 | 浙江华康药业股份有限公司 | Induction nucleation crystallization method for improving anti-caking performance of xylitol |
| CN116063158B (en) * | 2022-12-17 | 2024-05-10 | 浙江华康药业股份有限公司 | Induction nucleation crystallization method for improving anti-caking performance of xylitol |
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Application publication date: 20220107 |