CN104498559A - Clean production process of xylose - Google Patents
Clean production process of xylose Download PDFInfo
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- CN104498559A CN104498559A CN201410701716.4A CN201410701716A CN104498559A CN 104498559 A CN104498559 A CN 104498559A CN 201410701716 A CN201410701716 A CN 201410701716A CN 104498559 A CN104498559 A CN 104498559A
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Abstract
The invention provides a clean production process of xylose. The clean production process of xylose mainly comprises the following steps of: pretreating, namely steaming and exploding; hydrolyzing with an enzyme; refining by separating chromatographically; concentrating continuously with a membrane; and concentrating by evaporating steam. Due to the adoption of the clean production process of xylose, the problems in the prior art that sewage contains sulfate ions and can not be treated biochemically can be solved, and the problems of high consumption of water, acids, alkalis and energy, large discharge amount of wastewater, serious pollution to environment, high cost and long production cycle can be also solved.
Description
Technical field
The invention belongs to technical field of functional sugar production, be specifically related to a kind of preparation technology of cleaner production wood sugar.
Background technology
Xylose product is white crystals or crystalline powder, and taste is sweet, and sugariness is equivalent to 70% of sucrose, there is no Energy value, heat can not be provided for human body, to the bifidus bacillus in human intestinal, there is higher increment effect, the micro-ecological environment of human body can be improved, improve immunity of organisms.Xylose product is mainly used in producing Xylitol, add at food-processing, beverage, pet food is widely used in preparing etc., also can be used as meat product, cereal product flavor-improving agent and prepare the raw material of meat flavoring, high-grade color of soy sauce, to the quality of the life improving people, there is critical function and effect.
Tradition preparation xylose product is with agroforestry wastes such as corn cob, bagasse, mao bamboon slag, Cortex Betulae Luminiferaes for raw material, is prepared from through operations such as pre-treatment, sulphuric acid hydrolysis, light calcium carbonate neutralization, powder activity carbon decoloring, the exchange of positive negative and positive primary ions, primary steam evaporation concentration, negative and positive the moon Two-step ion-exchanging, secondary steam evaporation concentration, single-effect evaporation, crystallization, centrifugal, oven dry.Owing to adopting sulphuric acid hydrolysis in this technique, therefore in the waste water of hydrolyzed solution and discharge containing a large amount of sulfate ions, very large restraining effect is had to the anerobe of wastewater treatment, according to verification experimental verification, often containing the sulfate ion of a mole, the anerobe of ten moles can be suppressed active, cause this waste water to be difficult to process.Owing to adopting the SO in anion and cation exchange resin removal feed liquid
4 2-, Cl
-deng negatively charged ion and Ca
2+, Mg
2+, Na
+deng positively charged ion, refining purification liquid glucose, greatly, water consumption is large for this technique ubiquity acid, quantity of alkali consumption, and the wastewater flow rate of generation is also very large, and the problems such as production cost is high, are unfavorable for the Sustainable development of industry.Simultaneously, because wood sugar feed liquid also exists the low problem of concentration, this feed liquid, after repeatedly refining from friendship, all reduces concentration, and concentration when reach final crystallization needs to consume a large amount of steam, as can be seen here, traditional xylose production process also exists the three high problems such as high flow rate, high energy consumption, high pollution, does not meet national industrial policies, there is larger industry development risk, therefore, the technique researching and developing a kind of cleaner production wood sugar is that situation become.
About the research of the agriculture and forestry organic waste material hydrolysis processs such as corn cob, bagasse, mao bamboon slag, Cortex Betulae Luminiferae, someone attempts adopting oxalic acid to replace sulfuric acid to be hydrolyzed to agriculture and forestry organic waste material as hydrolyst, this technique solves the problem of the difficult biochemical treatment of waste water, but because oxalic acid is more much higher than sulfuric acid price, cause the production cost of wood sugar very high, enterprise cannot bear.The refining purifying technique of Xylose, someone adopts the method for electrodialysis depickling desalination to reduce the specific conductivity of feed liquid, reach refining object of purifying, but because Xylose is often impure, complicated component, seriously polluted to electrodialytic membranes, cause the work-ing life of film short, efficiency is low, and industrialization difficulty is very large.
Summary of the invention
The object of this invention is to provide a kind of technique of cleaner production wood sugar, contain sulfate ion, not easily biochemical treatment to solve sewage in prior art, water loss is large, acid, alkali consume high, and energy consumption is high, and wastewater discharge is large, the problems such as contaminate environment is serious, and cost is high, and the production cycle is long.
Technique of the present invention, comprises the following steps:
(1) steam quick-fried pre-treatment: get agriculture and forestry organic waste material and put into and steam quick-fried equipment, be warming up to 200-250 DEG C, after insulation 60-150 second, material is produced;
(2) enzymolysis: will import in enzymatic vessel through steaming quick-fried pretreated material, add water by the 1:5-1:15 of agriculture and forestry organic waste material dry weight, adjust pH is 3.0-5.0, and hierarchy of control temperature is 30-50 DEG C, hemicellulase is added, enzymolysis 10-50 hour by the 1-10% of agriculture and forestry organic waste material dry weight;
(3) filtering separation: adopt flame filter press to filter, collect filtrate, obtain Xylose;
(4) chromatographic refining is separated: adopt chromatographic separation polymeric adsorbent to carry out refiningly obtaining the wood sugar that dry concentration is 3-5%, specific conductivity is 200-1000us/cm, transmittance is 70-90%, xylose purity is 70-85% and refining purification liquid to Xylose;
(5) continuous film concentrates: adopt nanofiltration membrane or reverse osmosis membrane to refine purification liquid to wood sugar and concentrate, obtain wood sugar membrane concentration liquid, its dry concentration is 10-13%;
(6) steam raising concentrates: adopting multiple-effect steam vaporizer to carry out evaporation concentration to wood sugar membrane concentration liquid, is 80-85% to dry concentration;
(7) crystallization, centrifugal, oven dry: the mode adopting cooling crystallization, decrease temperature crystalline is carried out by the cooling rate of 0.8-1.2 DEG C/h, by whizzer, xylose crystals is separated with mother liquor, obtain xylose crystals, finally by steam drying device by the moisture removal in xylose crystals, obtain crystalline xylose.
Agriculture and forestry organic waste material of the present invention is all agriculture and forestry organic waste material resources containing Mierocrystalline cellulose, hemicellulose, lignin component.
Preferably, described agriculture and forestry organic waste material is corn cob, bagasse, mao bamboon slag, maize straw, wheat-straw, straw, reed, Cortex Betulae Luminiferae.
Hemicellulase of the present invention is mainly zytase, and its effect is that hemicellulose is decomposed into pentose, and the main component of pentose is wood sugar.
It is one in sodium form, potassium type, calcium type, Hydrogen, lead-type chromatographic separation polymeric adsorbent that chromatographic separation polymeric adsorbent of the present invention comprises model.
Preferably, described chromatographic separation polymeric adsorbent is Hydrogen chromatographic separation resin.
Further, the separation temperature that described step (4) chromatographic refining is separated controls at 30-40 DEG C.
Further, the separation temperature that described step (4) chromatographic refining is separated is 35 DEG C.
Test proves, in the temperature range that resin and feed liquid tolerate, temperature is higher, resolution is higher, and separating effect is better, and temperature is lower, the resolution of chromatographic separation resin is lower, and separating effect is poorer, when separation temperature is lower than 30 DEG C, the resolution of chromatographic separation resin obviously reduces, and causes magazins' layout not thorough, when temperature is higher than 40 DEG C, sex change, variable color can be there is in the impurity in feed liquid, not easily remove, it is aging to accelerate resin simultaneously, has a strong impact on resin life.When temperature is 35 DEG C, the resolution of chromatographic separation resin and resin life are best.
According to the present invention, before the film that described step (5) continuous film is concentrated, pressure is 2.5-3.0 Mpa, and after film, pressure is 2.3-2.8 Mpa, and before film, after pressure and film, pressure difference is 0.18-0.22 Mpa.
Test proves, during continuous film is concentrated, before film, after pressure and film, pressure difference is 0.18-0.22 Mpa, can ensure that the dry concentration of the wood sugar membrane concentration liquid obtained is 10-13%, significantly can reduce the consumption of steam in steam raising enrichment step, reduce costs.
Multiple-effect steam vaporizer of the present invention refers to the one or more combination in double-effect evaporator, triple-effect evaporator, quadruple effect evaporator, quintuple effect evaporator, single-effect evaporator.
The positively effect adopting present invention process to prepare xylose product is:
(1) adopt the quick-fried method for pretreating process agriculture and forestry organic waste material of steaming, greatly facilitate Mierocrystalline cellulose in agriculture and forestry organic waste material, hemicellulose is separated with lignin component, its dense structure is fully opened, is beneficial to the infiltration of enzyme, there is good hydrolysis result.This method for pretreating can faster production rhythm greatly simultaneously, reduces production cost, save equipment total price, reduce investment.
(2) hemicellulose in hemicellulase enzymolysis agriculture and forestry organic waste material is adopted to be the sulphuric acid hydrolysis that wood sugar replaces in traditional technology, there is mild condition, Xylose is of light color, side reaction is few, water consumption is few, the advantages such as wastewater discharge is few, the easy biochemical treatment of waste water, meet the cleaner production requirement that country advocates.
(3) chromatographic separation technology is adopted to replace traditional ion exchange resin to refine purifying xylose liquid, not consumption acids, alkali, produce without regenerating spent acid buck, the advantages such as have separation efficiency high, water consumption is few, and wastewater discharge is few, simultaneously in conjunction with continuous film concentration technology technology, significantly can reduce steam consumption, there is good energy-saving and water-saving effect, there is far-reaching environment protection significance and social effect.
(4) Technology of the present invention is compared to the Technology of traditional xylose production, simplifies technical process, shortens the production cycle, reduces the production cost of wood sugar, decreases discharge of wastewater, has significant economy, environment protecting.
Embodiment
Below in conjunction with specific embodiment, the present invention is described further.
embodiment one
1, steam quick-fried pre-treatment: get the quick-fried equipment of steaming that 800g corn cob puts into 5 liters, be warming up to 200 DEG C, be incubated after 150 seconds, spurt rapidly, obtain steaming quick-fried corn cob slurry mud.
2, enzymolysis: 3000g is steamed quick-fried corn cob slurry mud (dry corn cob is about 600g) and import in the enzymatic vessel of 10 liters, service water 4200g is added by the 1:5 of corn cob dry, be 3.0 with 30% hydrochloric acid adjust pH, control temperature is 50 DEG C, add compound hemicellulase 160g, when constantly stirring, enzymolysis 50 hours, make hemicellulose components wherein be converted into the wood sugar of individual molecule, obtain the mixture of Xylose and slag.
3, filtering separation: adopt flame filter press to be separated with slag by Xylose, obtain Xylose 5400g, its dry concentration is 8%, and xylose purity is 59.8%, and transmittance is 2%, and specific conductivity is 20000us/cm.
4, chromatographic refining is separated: squeezed into by Xylose in the chromatographic separation device that 10 liters of sodium form chromatographic separation polymeric adsorbents are housed, control that separation temperature is 40 DEG C, magnetic valve switching time is 100 seconds, charging flow velocity is 5 ls/h, carry out continuous chromatography lock out operation, remove the impurity such as pigment, zwitterion wherein, obtain refining purifying xylose liquid, its index is: dry concentration is 5%, xylose purity is 85%, transmittance is 70%, specific conductivity is 1000us/cm.
5, continuous film concentrates: passed into by chromatographic separation refined xylose liquid and be equipped with in the continuous film concentrating device system of nanofiltration membrane, before controlling diaphragm, pressure is that after 3.0MPa, film, pressure is 2.8MPa, charging flow velocity is 10 ls/h, obtain dry concentration be 13% wood sugar membrane concentration liquid and dry concentration be 0 film water-dialyzing liquid.Film water-dialyzing liquid, can turn back to " enzymolysis " operation, recycle again.
6, steam raising concentrates: adopt triple-effect evaporator by dry concentration be 13% wood sugar membrane concentration liquid evaporation concentration be 50% to dry concentration, and then adopt single-effect evaporator by dry concentration be 50% Xylose to be concentrated into dry concentration be 80%.
7, crystallization, centrifugal, oven dry: decrease temperature crystalline is carried out to wood sugar massecuite by the speed of 1 DEG C/h, xylose crystals is separated out, by supercentrifuge, xylose crystals is separated with mother liquor, obtain xylose crystals, last under the condition of 70 DEG C, adopt the dryer of fluidized bed type to be dried to moisture content below 1% by xylose crystals, obtain finished product crystalline xylose.
embodiment two
1, quick-fried pre-treatment is steamed: get the quick-fried equipment of steaming that 500g bagasse puts into 5 liters, be warming up to 250 DEG C, be incubated after 60 seconds, spurt rapidly, obtain steaming quick-fried bagasse pulp mud.
2, enzymolysis: 2500g is steamed quick-fried bagasse pulp mud (dry bagasse is about 350g) and import in the enzymatic vessel of 10 liters, service water 6300g is added by the 1:10 of bagasse dry, be 5.0 with 30% hydrochloric acid adjust pH, control temperature is 30 DEG C, add zytase 8g, when constantly stirring, enzymolysis 10 hours, make hemicellulose components wherein be converted into the wood sugar of individual molecule, obtain the mixture of Xylose and slag.
3, filtering separation: adopt flame filter press to be separated with slag by Xylose, obtain Xylose 7500g, its dry concentration is 5%, and xylose purity is 40.5%, and transmittance is 10%, and specific conductivity is 10000us/cm.
4, chromatographic refining is separated: squeezed into by Xylose in the chromatographic separation device that 10 liters of potassium type chromatographic separation polymeric adsorbents are housed, control that separation temperature is 38 DEG C, magnetic valve switching time is 400 seconds, charging flow velocity is 15 ls/h, carry out continuous chromatography lock out operation, remove the impurity such as pigment, zwitterion wherein, obtain refining purifying xylose liquid, its index is: dry concentration is 3%, xylose purity is 70%, transmittance is 90%, specific conductivity is 200us/cm.
5, continuous film concentrates: passed into by chromatographic separation refined xylose liquid and be equipped with in the continuous film concentrating device system of reverse osmosis membrane, before controlling diaphragm, pressure is that after 2.8MPa, film, pressure is 2.5MPa, charging flow velocity is 5 ls/h, obtain dry concentration be 10% wood sugar membrane concentration liquid and dry concentration be 0 film water-dialyzing liquid.Film water-dialyzing liquid, can turn back to " enzymolysis " operation, recycle again.
6, steam raising concentrates: adopt quadruple effect evaporator by dry concentration be 10% wood sugar membrane concentration liquid evaporation concentration be 85% to dry concentration.
7, crystallization, centrifugal, oven dry: decrease temperature crystalline is carried out to wood sugar massecuite by the speed of 1 DEG C/h, xylose crystals is separated out, by supercentrifuge, xylose crystals is separated with mother liquor, obtain xylose crystals, last under the condition of 70 DEG C, adopt the dryer of fluidized bed type to be dried to moisture content below 1% by xylose crystals, obtain finished product crystalline xylose.
embodiment three
1, steam quick-fried pre-treatment: get the quick-fried equipment of steaming that 700g mao bamboon slag puts into 5 liters, be warming up to 220 DEG C, be incubated after 120 seconds, spurt rapidly, obtain steaming quick-fried mao bamboon slag slurry mud.
2, enzymolysis: 2000g is steamed quick-fried mao bamboon slag slurry mud (dry mao bamboon slag is about 500g) and import in the enzymatic vessel of 10 liters, service water 6000g is added by the 1:15 of mao bamboon slag dry, be 4.5 with 30% sodium hydroxide adjust pH, control temperature is 40 DEG C, add compound hemicellulase 40g, when constantly stirring, enzymolysis 40 hours, make hemicellulose components wherein be converted into the wood sugar of individual molecule, obtain the mixture of Xylose and slag.
3, filtering separation: adopt flame filter press to be separated with slag by Xylose, obtain Xylose 7000g, its dry concentration is 5.5%, and xylose purity is 50%, and transmittance is 8%, and specific conductivity is 15000us/cm.
4, chromatographic refining is separated: squeezed into by Xylose in the chromatographic separation device that 10 liters of calcium type chromatographic separation polymeric adsorbents are housed, control that separation temperature is 30 DEG C, magnetic valve switching time is 300 seconds, charging flow velocity is 10 ls/h, carry out continuous chromatography lock out operation, remove the impurity such as pigment, zwitterion wherein, obtain refining purifying xylose liquid, its index is: dry concentration is 4%, xylose purity is 75%, transmittance is 80%, specific conductivity is 500us/cm.
5, continuous film concentrates: passed into by chromatographic separation refined xylose liquid and be equipped with in the continuous film concentrating device system of nanofiltration membrane, before controlling diaphragm, pressure is that after 2.5MPa, film, pressure is 2.3MPa, charging flow velocity is 7 ls/h, obtain dry concentration be 11% wood sugar membrane concentration liquid and dry concentration be 0 film water-dialyzing liquid.Film water-dialyzing liquid, can turn back to " enzymolysis " operation, recycle again.
6, steam raising concentrates: adopt quintuple effect evaporator by dry concentration be 11% wood sugar membrane concentration liquid evaporation concentration be 55% to dry concentration, and then adopt single-effect evaporator by dry concentration be 55% Xylose to be concentrated into dry concentration be 81.5%.
7, crystallization, centrifugal, oven dry: decrease temperature crystalline is carried out to wood sugar massecuite by the speed of 1 DEG C/h, xylose crystals is separated out, by supercentrifuge, xylose crystals is separated with mother liquor, obtain xylose crystals, last under the condition of 75 DEG C, adopt the dryer of boiling type to be dried to moisture content below 1% by xylose crystals, obtain finished product crystalline xylose.
Claims (10)
1. a technique for cleaner production wood sugar, is characterized in that, comprises the following steps:
(1) steam quick-fried pre-treatment: get agriculture and forestry organic waste material and put into and steam quick-fried equipment, be warming up to 200-250 DEG C, after insulation 60-150 second, material is produced;
(2) enzymolysis: will import in enzymatic vessel through steaming quick-fried pretreated material, add water by the 1:5-1:15 of agriculture and forestry organic waste material dry weight, adjust pH is 3.0-5.0, and hierarchy of control temperature is 30-50 DEG C, hemicellulase is added, enzymolysis 10-50 hour by the 1-10% of agriculture and forestry organic waste material dry weight;
(3) filtering separation: adopt flame filter press to filter, collect filtrate, obtain Xylose;
(4) chromatographic refining is separated: adopt chromatographic separation polymeric adsorbent to carry out refiningly obtaining the wood sugar that dry concentration is 3-5%, specific conductivity is 200-1000us/cm, transmittance is 70-90%, xylose purity is 70-85% and refining purification liquid to Xylose;
(5) continuous film concentrates: adopt nanofiltration membrane or reverse osmosis membrane to refine purification liquid to wood sugar and concentrate, obtain wood sugar membrane concentration liquid, its dry concentration is 10-13%;
(6) steam raising concentrates: adopting multiple-effect steam vaporizer to carry out evaporation concentration to wood sugar membrane concentration liquid, is 80-85% to dry concentration;
(7) crystallization, centrifugal, oven dry: the mode adopting cooling crystallization, decrease temperature crystalline is carried out by the cooling rate of 0.8-1.2 DEG C/h, by whizzer, xylose crystals is separated with mother liquor, obtain xylose crystals, finally by steam drying device by the moisture removal in xylose crystals, obtain crystalline xylose.
2. technique as claimed in claim 1, it is characterized in that, described agriculture and forestry organic waste material is all agriculture and forestry organic waste material resources containing Mierocrystalline cellulose, hemicellulose, lignin component.
3. technique as claimed in claim 2, it is characterized in that, described agriculture and forestry organic waste material is corn cob, bagasse, mao bamboon slag, maize straw, wheat-straw, straw, reed, Cortex Betulae Luminiferae.
4. technique as claimed in claim 1, it is characterized in that, described hemicellulase is zytase.
5. technique as claimed in claim 1, is characterized in that, it is one in sodium form, potassium type, calcium type, Hydrogen, lead-type chromatographic separation polymeric adsorbent that described chromatographic separation polymeric adsorbent comprises model.
6. technique as claimed in claim 5, it is characterized in that, described chromatographic separation polymeric adsorbent is Hydrogen chromatographic separation resin.
7. technique as described in any one of claim 1,5,6, is characterized in that, the separation temperature that described step (4) chromatographic refining is separated controls at 30-40 DEG C.
8. technique as claimed in claim 7, is characterized in that, the separation temperature that described step (4) chromatographic refining is separated is 35 DEG C.
9. technique as claimed in claim 1, is characterized in that, before the film that described step (5) continuous film is concentrated, pressure is 2.5-3.0 Mpa, and after film, pressure is 2.3-2.8 Mpa, and before film, after pressure and film, pressure difference is 0.18-0.22 Mpa.
10. technique as claimed in claim 1, it is characterized in that, described multiple-effect steam vaporizer refers to the one or more combination in double-effect evaporator, triple-effect evaporator, quadruple effect evaporator, quintuple effect evaporator, single-effect evaporator.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105695325A (en) * | 2016-04-01 | 2016-06-22 | 张喜强 | Device and method for extracting xylitol and chlorophyll dietary fiber from whole-plant corn straws |
| CN106191328A (en) * | 2016-09-23 | 2016-12-07 | 邵荣珠 | A kind of xylose production process |
| CN109452505A (en) * | 2018-12-29 | 2019-03-12 | 广西壮族自治区农业科学院农产品质量安全与检测技术研究所 | A kind of sugar-cane juice preparation method of high Xylose Content |
| CN109761755A (en) * | 2019-03-18 | 2019-05-17 | 浙江华康药业股份有限公司 | Integrated evaporation, crystallization and centrifuge separation prepare the device and control method of xylitol |
| CN110042177A (en) * | 2019-05-08 | 2019-07-23 | 河北曌玉科技有限公司 | A kind of hydrolysis of hemicellulose prepares the method and system of xylose |
| CN110303024A (en) * | 2018-03-20 | 2019-10-08 | 郑庆义 | A kind of straw method of comprehensive utilization |
| CN111996296A (en) * | 2020-09-15 | 2020-11-27 | 无锡绿色分离应用技术研究所有限公司 | Environment-friendly method for extracting xylose from hemicellulose |
| CN112210575A (en) * | 2020-11-05 | 2021-01-12 | 浙江科技学院 | Process for preparing xylose by using tea leaves |
| CN113004346A (en) * | 2021-02-07 | 2021-06-22 | 济南茂腾生物科技有限公司 | Method for preparing xylose by negative pressure coupling normal pressure crystallization |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105695325A (en) * | 2016-04-01 | 2016-06-22 | 张喜强 | Device and method for extracting xylitol and chlorophyll dietary fiber from whole-plant corn straws |
| CN106191328A (en) * | 2016-09-23 | 2016-12-07 | 邵荣珠 | A kind of xylose production process |
| CN110303024A (en) * | 2018-03-20 | 2019-10-08 | 郑庆义 | A kind of straw method of comprehensive utilization |
| CN109452505A (en) * | 2018-12-29 | 2019-03-12 | 广西壮族自治区农业科学院农产品质量安全与检测技术研究所 | A kind of sugar-cane juice preparation method of high Xylose Content |
| CN109761755A (en) * | 2019-03-18 | 2019-05-17 | 浙江华康药业股份有限公司 | Integrated evaporation, crystallization and centrifuge separation prepare the device and control method of xylitol |
| CN110042177A (en) * | 2019-05-08 | 2019-07-23 | 河北曌玉科技有限公司 | A kind of hydrolysis of hemicellulose prepares the method and system of xylose |
| CN111996296A (en) * | 2020-09-15 | 2020-11-27 | 无锡绿色分离应用技术研究所有限公司 | Environment-friendly method for extracting xylose from hemicellulose |
| CN112210575A (en) * | 2020-11-05 | 2021-01-12 | 浙江科技学院 | Process for preparing xylose by using tea leaves |
| CN113004346A (en) * | 2021-02-07 | 2021-06-22 | 济南茂腾生物科技有限公司 | Method for preparing xylose by negative pressure coupling normal pressure crystallization |
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