CN112479813A - Production process of xylitol - Google Patents
Production process of xylitol Download PDFInfo
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- CN112479813A CN112479813A CN202011238724.1A CN202011238724A CN112479813A CN 112479813 A CN112479813 A CN 112479813A CN 202011238724 A CN202011238724 A CN 202011238724A CN 112479813 A CN112479813 A CN 112479813A
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- xylitol
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- ion exchange
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- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 title claims abstract description 59
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 239000000811 xylitol Substances 0.000 title claims abstract description 59
- 235000010447 xylitol Nutrition 0.000 title claims abstract description 59
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 title claims abstract description 59
- 229960002675 xylitol Drugs 0.000 title claims abstract description 59
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 47
- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 claims abstract description 30
- 238000001704 evaporation Methods 0.000 claims abstract description 19
- 230000008020 evaporation Effects 0.000 claims abstract description 16
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 claims abstract description 15
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000005342 ion exchange Methods 0.000 claims abstract description 15
- 238000002425 crystallisation Methods 0.000 claims abstract description 13
- 230000008025 crystallization Effects 0.000 claims abstract description 13
- 239000007787 solid Substances 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000004806 packaging method and process Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 45
- 239000007788 liquid Substances 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000012452 mother liquor Substances 0.000 claims description 14
- 239000013078 crystal Substances 0.000 claims description 13
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 9
- 238000000926 separation method Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 239000003957 anion exchange resin Substances 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 6
- 150000002500 ions Chemical class 0.000 claims description 6
- 239000003729 cation exchange resin Substances 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 5
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 4
- 239000003456 ion exchange resin Substances 0.000 claims description 4
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 4
- 229910001453 nickel ion Inorganic materials 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229910000838 Al alloy Inorganic materials 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 claims description 2
- 229910021645 metal ion Inorganic materials 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 2
- 238000005119 centrifugation Methods 0.000 abstract 1
- 239000012141 concentrate Substances 0.000 abstract 1
- 238000004042 decolorization Methods 0.000 abstract 1
- 238000004090 dissolution Methods 0.000 abstract 1
- 238000005984 hydrogenation reaction Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 4
- 239000003463 adsorbent Substances 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000000413 hydrolysate Substances 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 235000001674 Agaricus brunnescens Nutrition 0.000 description 1
- 108010009736 Protein Hydrolysates Proteins 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 235000003599 food sweetener Nutrition 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000003765 sweetening agent Substances 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 230000004127 xylose metabolism Effects 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/132—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group
- C07C29/136—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group of >C=O containing groups, e.g. —COOH
- C07C29/14—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group of >C=O containing groups, e.g. —COOH of a —CHO group
- C07C29/141—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group of >C=O containing groups, e.g. —COOH of a —CHO group with hydrogen or hydrogen-containing gases
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the technical field of sugar industry by utilizing natural resources, and particularly discloses a production process of xylitol, which sequentially comprises the steps of xylose dissolution → material preparation → hydrogenation → mixing → decolorization → ion exchange → evaporation → crystallization → centrifugation → drying and the like to obtain solid crystalline xylitol, and a finished product is formed by packaging. The invention alcoholizes the xylose to concentrate the xylitol, the process has high xylitol crystallization rate, more satisfactory purity, less energy consumption, more reasonable process, effectively reduced labor intensity of workers, greatly reduced processing cost and better solved the problem of lagging process for preparing the xylitol.
Description
Technical Field
The invention relates to the technical field of sugar industry by utilizing natural resources, in particular to a production process of xylitol.
Background
Xylitol is a five-carbon sugar alcohol, a normal intermediate product of xylose metabolism, is in the form of crystalline white powder, and is widely found in foods such as fruits, vegetables, cereals, mushrooms, and plants such as wood, straw, corncob, and the like. It can be used as sweetening agent, nutrient and medicine, and can be extensively used in the fields of chemical industry, food and medicine, etc. At present, most of the processes for producing xylitol in China adopt a neutralization deacidification process. Namely, a neutralization method is adopted when the hydrolysate is purified. The process route of the method is that the raw materials are hydrolyzed, neutralized, decolored, ion exchanged, concentrated and the like to obtain the liquid xylitol with relatively high yield.
Disclosure of Invention
In view of the above, the invention aims to provide a xylitol production process, in which xylitol is alcoholized and concentrated into xylitol, the process has the advantages of high xylitol crystallization rate, more satisfactory purity, less energy consumption, more reasonable process, effectively reduced labor intensity of workers, greatly reduced processing cost and better solved the problem of lagging xylitol preparation process.
In order to achieve the purpose, the invention adopts the following technical scheme:
the production process of xylitol comprises the following steps:
1) dissolving xylose, namely respectively adding raw material crystalline xylose and hot process water to dissolve the raw material crystalline xylose and the hot process water to form a xylose aqueous solution with the concentration of 50-55 percent;
2) preparing materials, namely adding a material preparing tank into the solution obtained in the step 1, and adding a certain amount of catalyst to form a mixed solution;
3) hydrogenating, adding hydrogen with a certain pressure into the solution obtained in the step 2, and heating to alcoholize the solution;
4) mixing, namely adding the solution obtained in the step 3 into hot process water and xylitol mother liquor to obtain a mixed solution with the concentration of 50-55%;
5) decoloring, namely adsorbing, filtering and decoloring the mixed solution obtained in the step 4 by a granular carbon column;
6) ion exchange, namely removing metal ions and other impurity ions from the solution obtained in the step 5 through ion exchange;
7) evaporating, namely performing double-effect evaporation and triple-effect evaporation on the solution obtained in the step 6 to enable the concentration of the solution to reach 70-75%;
8) crystallizing, namely continuously adding steam into the solution obtained in the step 7 for heating, and continuously increasing the concentration of the aqueous solution to 85% -90%;
9) performing centrifugal separation, namely adding the solid-liquid mixture obtained in the step 8 into a centrifugal separator for solid-liquid separation, wherein the separated liquid part is xylitol mother liquor, one part of the xylitol mother liquor is added into the step 4 for mixing, the other part of the xylitol mother liquor is subjected to decoloration, evaporation, cooling crystallization and centrifugal separation in sequence, the obtained solid is xylitol bicrystal, and the obtained liquid is filled to form commercial xylitol mother liquor with the concentration of 52.5%; the xylitol bicrystal is used for being put into the step 4 and mixed to obtain a xylitol solution with required concentration;
10) and (3) drying, namely heating and drying the solid part separated in the step (9) to obtain solid crystal xylitol, and packaging to form a finished product.
Preferably, the catalyst in step 3 is magnesium powder and/or nickel-aluminum alloy.
Preferably, in step 6, the ion exchange deacidification process is to remove nickel ions and other impurity ions by using ion exchange resin through an ion exchange method, and comprises three times of exchange, wherein the first exchange is performed by using cation exchange resin, the second exchange is performed by using anion exchange resin, and the third exchange is performed by using mixed bed exchange, namely, by using cation exchange resin and anion exchange resin.
Preferably, the double-effect evaporation process in the step 7 is to heat the solution to increase the concentration of the solution to 55-60% at a temperature of 80 ℃.
Preferably, the triple effect evaporation process of step 7 is to increase the concentration of the solution to 70% -75% at 65 ℃ by heating the solution.
Preferably, in the crystallization process described in step 8, in order to promote crystal development, a seed crystal can be added into the aqueous solution for crystallization assistance.
Preferably, in step 8, the seed crystal is xylitol grinding powder.
The invention has the beneficial effects that:
the process has the advantages of high xylitol crystallization rate, more satisfactory purity, less energy consumption, more reasonable process, effective reduction of labor intensity of workers, great reduction of processing cost and better solution of the problem of lagging process for preparing xylitol.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic process flow diagram of the present invention.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in figure 1, the production process of xylitol comprises the following steps:
1) dissolving xylose, namely respectively adding raw material crystalline xylose and hot process water to dissolve the raw material crystalline xylose and the hot process water to form a xylose aqueous solution with the concentration of 50-55 percent;
2) preparing materials, namely adding the solution obtained in the step 1 into a material preparing tank, and adding a certain amount of catalyst to form a mixed solution;
3) hydrogenating, namely injecting the solution obtained in the step 2 into a reaction kettle, adding hydrogen with certain pressure, and heating to alcoholize the solution; in the process, the carbonyl of the xylose is hydrogenated and reduced into hydroxyl under the action of a catalyst in the environment of 4-4.5MPa and 80-120 ℃.
4) Mixing, namely adding the solution obtained in the step 3 into hot process water and xylitol mother liquor to obtain a mixed solution with the concentration of 50% -55%;
5) decoloring, namely adsorbing, filtering and decoloring the mixed solution obtained in the step 4 by a granular carbon column; the xylitol hydrolysate is decolorized mainly by adsorption, the adsorbent is porous and has a large specific surface area, and the adsorbent is widely used, such as clay, sulfonated coal, pyrolignin and activated carbon, wherein the activated carbon is relatively extensive.
6) Ion exchange, namely deacidifying the solution obtained in the step 5 through ion exchange; the ion exchange deacidification process is to remove nickel ions and other impurity ions by using ion exchange resin by using an ion exchange method, so that the quality of the purified liquid is improved, and the quality of the product is further improved. In the process, three exchanges are included totally, the meaning of each exchange is different, so that the adopted ion exchange resins are different, the first exchange is mainly used for removing nickel ions in the hydrolysate, so that cation exchange is adopted, anion exchange resin is adopted for the second exchange, mixed bed exchange is adopted for the third exchange, namely, cation and anion exchange resins are adopted, and cation resin is also used singly. The ion exchange process improves the utilization rate and the service life of equipment, improves the quality of hydrogenated liquid and correspondingly improves the quality of products.
7) Evaporating, namely performing double-effect evaporation and triple-effect evaporation on the solution obtained in the step 6 to enable the concentration of the solution to reach 70-75%; in the process, in the double-effect evaporation process, the solution is heated to improve the concentration of the solution to 55-60% at the temperature of 80 ℃; the solution was then increased to 70-75% concentration at 65 ℃ by heating the solution during triple effect evaporation. The working principle of the double-effect evaporator is that the secondary steam generated by the first evaporator is used as a heating source again, the secondary steam is introduced into the other evaporator, an intelligent automatic control system is adopted to control the pressure and the boiling point of the solution in the evaporators to be properly reduced, the secondary steam generated by the first evaporator can be used for heating, and in the process, the condensation position of the first evaporator is the heating position of the second evaporator. In the same way, the triple-effect evaporator is based on the double-effect evaporator, and then introduces an evaporator, and takes the steam generated by the second evaporator as the heat source.
8) Crystallizing, namely continuously adding steam into the solution obtained in the step 7 for heating, and continuously increasing the concentration of the aqueous solution to 85-90%; in the process, crystal seeds which are xylitol grinding powder can be added into the aqueous solution for assisting crystallization in order to promote crystal growth, and the purpose of injection is to ensure that xylitol in the solution is attached to the crystal seeds so as to facilitate crystallization of larger xylitol crystals.
9) Performing centrifugal separation, namely adding the solid-liquid mixture obtained in the step 8 into a centrifugal separator for solid-liquid separation, wherein the separated liquid part is xylitol mother liquor, the xylitol mother liquor is subjected to decoloration, evaporation, cooling crystallization and centrifugal separation in sequence, the obtained solid is xylitol bicrystal, and the obtained liquid is filled to form commercial xylitol mother liquor with the concentration of 52.5%; and (4) putting the xylitol bicrystal into the step (4), and mixing to obtain a xylitol solution with the required concentration.
10) And (3) drying, namely heating and drying the solid part separated in the step (9) to obtain solid crystal xylitol, and packaging to form a finished product.
It should be understood that the detailed description of the present invention is only for illustrating the present invention and is not limited by the technical solutions described in the embodiments of the present invention, and those skilled in the art should understand that the present invention can be modified or substituted equally to achieve the same technical effects; as long as the use requirements are met, the method is within the protection scope of the invention.
Claims (7)
1. The production process of the xylitol is characterized by comprising the following steps:
1) dissolving xylose, namely respectively adding raw material crystalline xylose and hot process water to dissolve the raw material crystalline xylose and the hot process water to form a xylose aqueous solution with the concentration of 50-55 percent;
2) preparing materials, namely adding the solution obtained in the step 1 into a material preparing tank, and adding a certain amount of catalyst to form a mixed solution;
3) hydrogenating, adding hydrogen with a certain pressure into the solution obtained in the step 2, and heating to alcoholize the solution;
4) mixing, namely adding the solution obtained in the step 3 into hot process water and xylitol mother liquor to obtain a mixed solution with the concentration of 50-55%;
5) decoloring, namely adsorbing, filtering and decoloring the mixed solution obtained in the step 4 by a granular carbon column;
6) ion exchange, namely removing metal ions and other impurity ions from the solution obtained in the step 5 through ion exchange;
7) evaporating, namely performing double-effect evaporation and triple-effect evaporation on the solution obtained in the step 6 to enable the concentration of the solution to reach 70-75%;
8) crystallizing, namely continuously adding steam into the solution obtained in the step 7 for heating, and continuously increasing the concentration of the aqueous solution to 85% -90%;
9) performing centrifugal separation, namely adding the solid-liquid mixture obtained in the step 8 into a centrifugal separator for solid-liquid separation, wherein the separated liquid part is xylitol mother liquor, one part of the xylitol mother liquor is added into the step 4 for mixing, the other part of the xylitol mother liquor is subjected to decoloration, evaporation, cooling crystallization and centrifugal separation in sequence, the obtained solid is xylitol bicrystal, and the obtained liquid is filled to form commercial xylitol mother liquor with the concentration of 52.5%; the xylitol bicrystal is used for being put into the step 4 and mixed to obtain a xylitol solution with required concentration;
10) and (3) drying, namely heating and drying the solid part separated in the step (9) to obtain solid crystal xylitol, and packaging to form a finished product.
2. The process for producing xylitol according to claim 1, wherein: the catalyst in the step 3 is magnesium powder and/or nickel-aluminum alloy.
3. The process for producing xylitol according to claim 1, wherein: in step 6, the ion exchange deacidification process is to remove nickel ions and other impurity ions by using ion exchange resin through an ion exchange method, wherein the ion exchange deacidification process comprises three times of exchange, wherein the first exchange adopts cation exchange resin, the second exchange adopts anion exchange resin, and the third exchange adopts mixed bed exchange, namely, cation exchange resin and anion exchange resin.
4. The process for producing xylitol according to claim 1, wherein: the double-effect evaporation process in the step 7 is to heat the solution to raise the concentration of the solution to 55-60% at 80 ℃.
5. The process for producing xylitol according to claim 1 or 4, wherein: the triple effect evaporation process of step 7 is to heat the solution to raise the concentration of the solution to 70-75% at 65 ℃.
6. The process for producing xylitol according to claim 1, wherein: in the crystallization process in the step 8, in order to promote the crystal growth, seed crystals can be added into the aqueous solution for crystallization assistance.
7. The process for producing xylitol according to claim 6, wherein: in step 8, the seed crystal is xylitol grinding powder.
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Cited By (1)
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CN114149304A (en) * | 2021-12-27 | 2022-03-08 | 浙江华康药业股份有限公司 | Multistage xylitol mother liquor crystallization system and method thereof |
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