CN108484798A - A kind of methanol mediates the hydrophobic method efficiently separated with reuse alkaline solution and its dissolve hemicellulose - Google Patents
A kind of methanol mediates the hydrophobic method efficiently separated with reuse alkaline solution and its dissolve hemicellulose Download PDFInfo
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 title claims abstract description 180
- 229920002488 Hemicellulose Polymers 0.000 title claims abstract description 62
- 239000012670 alkaline solution Substances 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 18
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 29
- 238000000926 separation method Methods 0.000 claims abstract description 25
- 238000011084 recovery Methods 0.000 claims abstract description 19
- 230000001404 mediated effect Effects 0.000 claims abstract description 14
- 239000002244 precipitate Substances 0.000 claims abstract description 10
- 238000002309 gasification Methods 0.000 claims abstract description 7
- 239000012528 membrane Substances 0.000 claims abstract description 4
- 238000005119 centrifugation Methods 0.000 claims abstract description 3
- 238000001914 filtration Methods 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 239000003513 alkali Substances 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 9
- 239000006228 supernatant Substances 0.000 claims description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 229920001221 xylan Polymers 0.000 claims description 5
- 150000004823 xylans Chemical class 0.000 claims description 5
- LUEWUZLMQUOBSB-FSKGGBMCSA-N (2s,3s,4s,5s,6r)-2-[(2r,3s,4r,5r,6s)-6-[(2r,3s,4r,5s,6s)-4,5-dihydroxy-2-(hydroxymethyl)-6-[(2r,4r,5s,6r)-4,5,6-trihydroxy-2-(hydroxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-4,5-dihydroxy-2-(hydroxymethyl)oxan-3-yl]oxy-6-(hydroxymethyl)oxane-3,4,5-triol Chemical compound O[C@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@@H](O[C@@H]2[C@H](O[C@@H](OC3[C@H](O[C@@H](O)[C@@H](O)[C@H]3O)CO)[C@@H](O)[C@H]2O)CO)[C@H](O)[C@H]1O LUEWUZLMQUOBSB-FSKGGBMCSA-N 0.000 claims description 3
- 229920002581 Glucomannan Polymers 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 229940046240 glucomannan Drugs 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 2
- 239000000920 calcium hydroxide Substances 0.000 claims description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 2
- 238000010908 decantation Methods 0.000 claims description 2
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 238000001704 evaporation Methods 0.000 abstract description 3
- 230000008020 evaporation Effects 0.000 abstract description 3
- 230000036571 hydration Effects 0.000 abstract 1
- 238000006703 hydration reaction Methods 0.000 abstract 1
- 238000002955 isolation Methods 0.000 abstract 1
- 229920002521 macromolecule Polymers 0.000 abstract 1
- 238000004062 sedimentation Methods 0.000 abstract 1
- 238000005292 vacuum distillation Methods 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 30
- 238000001556 precipitation Methods 0.000 description 7
- 239000000835 fiber Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 229920002678 cellulose Polymers 0.000 description 3
- 239000001913 cellulose Substances 0.000 description 3
- 238000010907 mechanical stirring Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229920000297 Rayon Polymers 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 229920000057 Mannan Polymers 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 239000003495 polar organic solvent Substances 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 150000004804 polysaccharides Chemical class 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
- B01D36/04—Combinations of filters with settling tanks
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
- B01D36/04—Combinations of filters with settling tanks
- B01D36/045—Combination of filters with centrifugal separation devices
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F21/00—Dissolving
- B01F21/02—Methods
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- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Engineering & Computer Science (AREA)
- Molecular Biology (AREA)
- Materials Engineering (AREA)
- General Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
本发明公开了一种甲醇介导疏水高效分离与回用碱性溶液及其溶解半纤维素的方法，向溶解半纤维素的碱性溶液中加入甲醇并充分混匀，通过甲醇介导的疏水作用破坏半纤维素大分子与碱性溶液之间形成的水化层作用，使半纤维素从溶液体系中析出，并经沉降、离心或过滤分离得到半纤维素沉淀物与碱性甲醇溶液；利用碱性条件对甲醇与水蒸发和气化分离的促进作用，采用减压蒸（精）馏或气化膜完全分离甲醇与碱性溶液，所制得的碱性溶液、甲醇再回用于溶解半纤维素及分离。通过本方法的强碱性溶液、甲醇的完全回用，实现碱溶解与分离半纤维素的高效、清洁和节约化生产，碱溶解半纤维素的分离与回收效率超过99%。The invention discloses a methanol-mediated hydrophobic high-efficiency separation and reuse of alkaline solution and a method for dissolving hemicellulose. Methanol is added to the alkaline solution for dissolving hemicellulose and fully mixed. Through the methanol-mediated hydrophobic The effect destroys the hydration layer formed between the hemicellulose macromolecule and the alkaline solution, so that the hemicellulose is precipitated from the solution system, and separated by sedimentation, centrifugation or filtration to obtain hemicellulose precipitate and alkaline methanol solution; Using alkaline conditions to promote the evaporation and gasification separation of methanol and water, use vacuum distillation (rectification) or gasification membrane to completely separate methanol and alkaline solution, and the prepared alkaline solution and methanol are reused for dissolving Hemicellulose and its isolation. Through the complete reuse of strong alkaline solution and methanol in the method, efficient, clean and economical production of alkali-dissolved and separated hemicellulose is realized, and the separation and recovery efficiency of alkali-dissolved hemicellulose exceeds 99%.
Description
技术领域technical field
本发明涉及制浆造纸、粘胶纤维、再生纤维以及含有木聚糖、葡萄糖甘露聚糖等半纤维素组分的生物质资源加工技术领域，特别涉及一种甲醇介导疏水高效分离与回用碱性溶液及其溶解半纤维素的方法。The invention relates to the technical field of pulp and papermaking, viscose fiber, regenerated fiber, and biomass resource processing containing hemicellulose components such as xylan and glucomannan, in particular to a methanol-mediated hydrophobic high-efficiency separation and reuse Alkaline solution and method for dissolving hemicellulose.
背景技术Background technique
半纤维素是质纤维类原料中除纤维素及少量果胶与淀粉以外的一类聚糖类物质，主要以木聚糖、葡萄糖和甘露聚糖作为主链组分，与纤维素和木质素通过复杂的物理或化学作用形成紧密的复合结构。在以木质纤维类原料制取纸浆、粘胶纤维、再生纤维、木聚糖等产品的生产过程中，一般使用质量浓度5%以上强碱性溶液如氢氧化钠、碳酸钠和液氨等从原料中溶解和分离出半纤维素组分，生成富含半纤维素的高粘度、强碱性溶液，需要有效分离或消减碱性溶液中的半纤维素以实现碱性溶液回用和获得半纤维素产品，进而减少碱耗、水耗、环境污染和降低生产成本。Hemicellulose is a kind of polysaccharides other than cellulose and a small amount of pectin and starch in fiber raw materials. It mainly uses xylan, glucose and mannan as the main chain components, and cellulose and lignin A tight composite structure is formed through complex physical or chemical actions. In the production process of pulp, viscose fiber, regenerated fiber, xylan and other products from lignocellulosic raw materials, strong alkaline solutions with a mass concentration of more than 5% such as sodium hydroxide, sodium carbonate and liquid ammonia are generally used The hemicellulose component is dissolved and separated from the raw material to generate a high-viscosity, strong alkaline solution rich in hemicellulose. It is necessary to effectively separate or reduce the hemicellulose in the alkaline solution to realize the reuse of the alkaline solution and obtain hemicellulose Cellulose products, thereby reducing alkali consumption, water consumption, environmental pollution and production costs.
发明内容Contents of the invention
发明目的：针对半纤维素碱性溶液难以高效分离与回用的问题，本发明的目的是提供一种甲醇介导疏水高效分离与回用碱性溶液及其溶解半纤维素的方法，充分利用甲醇对溶解于碱性溶液中半纤维素分离与沉淀的物化特性，以甲醇介导形成疏水效应，破坏半纤维素与碱性溶液之间的亲和效应，促使半纤维素从甲醇碱性溶液高效分离并原位沉淀析出，以实现半纤维素的高效分离与制备，半纤维素的回收率超过99%，甲醇碱性溶液中半纤维素的残留率低于0.2%；利甲醇在碱性水溶液中的蒸发与气化的物化特性，采用蒸（精）馏或气化膜以高效分离甲醇碱性溶液体系分别制得甲醇、碱性溶液，可完成回收甲醇，碱性溶液中甲醇残留率低于0.02%。Purpose of the invention: Aiming at the problem that it is difficult to efficiently separate and reuse hemicellulose alkaline solution, the purpose of the present invention is to provide a methanol-mediated hydrophobic high-efficiency separation and reuse of alkaline solution and a method for dissolving hemicellulose, making full use of The physical and chemical properties of methanol on the separation and precipitation of hemicellulose dissolved in alkaline solution, the formation of hydrophobic effect mediated by methanol, destroys the affinity effect between hemicellulose and alkaline solution, and promotes the hemicellulose from methanol alkaline solution High-efficiency separation and in-situ precipitation to achieve high-efficiency separation and preparation of hemicellulose, the recovery rate of hemicellulose exceeds 99%, and the residual rate of hemicellulose in methanol alkaline solution is less than 0.2%; The physical and chemical characteristics of evaporation and gasification in aqueous solution, using steam (rectification) distillation or gasification membrane to efficiently separate methanol alkaline solution system to obtain methanol and alkaline solution respectively, can complete the recovery of methanol, and the residual rate of methanol in alkaline solution Less than 0.02%.
技术方案：为了实现上述发明目的，本发明采用的技术方案如下：Technical solution: In order to realize the above-mentioned purpose of the invention, the technical solution adopted in the present invention is as follows:
一种甲醇介导疏水高效分离与回用碱性溶液及其溶解半纤维素的方法，包括以下步骤：A method for methanol-mediated hydrophobic high-efficiency separation and reuse of an alkaline solution and its dissolution of hemicellulose, comprising the following steps:
1）向溶解半纤维素的碱性溶液中加入甲醇，充分搅拌混匀，静置沉降；1) Add methanol to the alkaline solution in which the hemicellulose is dissolved, stir well, and let it settle;
2）固液分离步骤1）的体系，得到上清液为甲醇碱性溶液，沉淀物为半纤维素；2) In the system of solid-liquid separation step 1), the obtained supernatant is methanol alkaline solution, and the precipitate is hemicellulose;
3）采用蒸馏或精馏或气化膜分离甲醇碱性溶液分别得到甲醇、碱性溶液；3) Use distillation or rectification or gasification membrane to separate methanol alkaline solution to obtain methanol and alkaline solution respectively;
4）分离得到的碱性溶液、甲醇，再回用于半纤维素溶解与分离制备。4) The separated alkaline solution and methanol are reused for hemicellulose dissolution and separation preparation.
所述碱性溶液为氢氧化钠、氢氧化钾、氢氧化钙、碳酸钠、碳酸钾溶液中的任意一种或它们的混合液。The alkaline solution is any one of sodium hydroxide, potassium hydroxide, calcium hydroxide, sodium carbonate, potassium carbonate solution or their mixture.
所述半纤维素为来自于木聚糖或葡甘聚糖为主链的线性或体型中的任意一种或它们的混合。The hemicellulose is any one of the linear or bulky chains derived from xylan or glucomannan, or a mixture of them.
步骤1）中，甲醇与碱性溶液体积比为1~4：1。In step 1), the volume ratio of methanol to alkaline solution is 1-4:1.
步骤2）中，固液分离的方法为倾析、虹吸、溢流、过滤或离心以及它们的组合。In step 2), the method of solid-liquid separation is decantation, siphon, overflow, filtration or centrifugation and their combination.
步骤1）中，静置沉降5~30分钟。In step 1), let it settle for 5-30 minutes.
步骤2）中，半纤维素回收得率超过99%，甲醇碱性溶液中半纤维素的残留率低于0.5%；In step 2), the recovery rate of hemicellulose exceeds 99%, and the residual rate of hemicellulose in the methanol alkaline solution is less than 0.5%;
步骤3）中，甲醇回收率超过99%，碱性溶液中残留的甲醇浓度低于0.01%。In step 3), the methanol recovery rate exceeds 99%, and the residual methanol concentration in the alkaline solution is lower than 0.01%.
有益效果：与现有技术相比，采用本发明方法可以实现半纤维素与碱性溶液的高效分离与回用，无水耗且显著降低电耗和生产成本；与乙醇等其它极性有机溶剂相比，对半纤维素尤其是低分子量组分的分离与沉淀效果更好，甲醇的沸点显著降低且不与水形成共沸物，与碱性溶液的蒸发（精馏）与气化分离的效果更好且成本更低，具有很好的实用性。Beneficial effects: Compared with the prior art, the method of the present invention can realize the efficient separation and reuse of hemicellulose and alkaline solution, without water consumption and significantly reduce power consumption and production cost; and other polar organic solvents such as ethanol Compared with hemicellulose, especially the separation and precipitation of low molecular weight components are better, the boiling point of methanol is significantly lower and does not form an azeotrope with water, and it is separated from the evaporation (rectification) and gasification of alkaline solution The effect is better, the cost is lower, and the utility model has good practicability.
具体实施方式Detailed ways
下面结合具体实施例对本发明做进一步的说明。The present invention will be further described below in conjunction with specific embodiments.
实施例1Example 1
在反应罐中加入300mL半纤维素强碱性溶液（pH11.0，半纤维素质量浓度3.0%，氢氧化钠质量浓度17%），匀速流加750mL甲醇至混合均匀，在室温条件下静置15 min至沉淀完全。采用管式离心机于9000g离心力条件下离心分离剩余溶液5min得到沉淀物，采用200mL的70%甲醇溶液分2次洗涤沉淀物即得到半纤维素，半纤维的回收率达到99.2%；离心上清液为甲醇碱溶液，碱回收率达到98%。采用旋转蒸发仪，控制真空度100mbar和釜底料液温度55~64℃，以2℃水为冷凝介质精馏分离甲醇碱溶液，至甲醇质量回收率超过98.6%，碱溶液中甲醇残余质量浓度低于0.02%，所得到的甲醇溶液、强碱性溶液即可回用。Add 300mL hemicellulose strong alkaline solution (pH11.0, hemicellulose mass concentration 3.0%, sodium hydroxide mass concentration 17%) into the reaction tank, add 750mL methanol at a uniform speed until the mixture is uniform, and let it stand at room temperature 15 min until the precipitation is complete. Use a tubular centrifuge to centrifuge the remaining solution for 5 minutes under the condition of 9000g centrifugal force to obtain the precipitate. Use 200mL of 70% methanol solution to wash the precipitate twice to obtain hemicellulose, and the recovery rate of the hemifiber reaches 99.2%. The liquid is methanol alkali solution, and the alkali recovery rate reaches 98%. Use a rotary evaporator, control the vacuum degree of 100mbar and the temperature of the bottom liquid at 55~64°C, and use 2°C water as the condensing medium to rectify and separate the methanol alkali solution until the methanol mass recovery rate exceeds 98.6%, and the residual mass concentration of methanol in the alkali solution If it is less than 0.02%, the obtained methanol solution and strong alkaline solution can be reused.
实施例2Example 2
在锥底不锈钢反应罐中加入10L半纤维素强碱性溶液（pH13.8，半纤维素质量浓度4.0%，氢氧化钠质量浓度20%），启动机械搅拌装置，匀速流加30L甲醇至混合均匀，在室温条件下静置30min至沉淀完全。采用管式离心机于9000 g离心力条件下离心分离剩余溶液10min得到沉淀物，以6L的70%浓度甲酸溶液分2次洗涤沉淀物即得半纤维素，半纤维素回收率达到99.1%；离心上清液得甲醇碱溶液，碱回收率达到98%。采用填料精馏塔，控制真空度100mbar和釜底料液温度65~70℃，以2℃水为冷凝介质精馏分离甲醇碱溶液，至甲醇质量回收率超过98.4%，碱溶液中甲醇残余质量浓度低于0.05%，所得到的甲醇溶液、强碱性溶液即可回用。Add 10L hemicellulose strong alkaline solution (pH13.8, hemicellulose mass concentration 4.0%, sodium hydroxide mass concentration 20%) into the conical bottom stainless steel reaction tank, start the mechanical stirring device, and add 30L methanol at a constant speed until mixed Evenly, let it stand at room temperature for 30 minutes until the precipitation is complete. Use a tubular centrifuge to centrifuge the remaining solution for 10 minutes under the condition of 9000 g centrifugal force to obtain the precipitate, wash the precipitate twice with 6L of 70% formic acid solution to obtain hemicellulose, and the recovery rate of hemicellulose reaches 99.1%; centrifuge The supernatant was obtained as a methanol alkali solution, and the alkali recovery rate reached 98%. A packed rectification tower is used to control the vacuum degree of 100mbar and the temperature of the bottom liquid at 65~70°C, and use 2°C water as the condensing medium to rectify and separate the methanol alkali solution until the recovery rate of methanol exceeds 98.4%, and the residual mass of methanol in the alkali solution If the concentration is lower than 0.05%, the obtained methanol solution and strong alkaline solution can be reused.
对比例1Comparative example 1
在反应罐中加入300mL半纤维素强碱性溶液（pH11.0，半纤维素质量浓度3.0%，氢氧化钠质量浓度17%），启动机械搅拌装置，匀速流加300mL乙醇至混合均匀，在室温条件下静置30min至沉淀完全。利用吸管吸取上清液A至400mL，采用管式离心机于5844g离心力条件下离心分离剩余溶液60min得到沉淀物，以500mL乙醇溶液（乙醇与水初始体积比80%：20%）分两次洗涤、离心沉淀物得半纤维素，半纤维素回收率达91.4%；合并离心上清液得乙醇碱溶液，碱回收率达到95%。采用旋转蒸发仪，控制真空度100mbar和釜底料液温度60~62℃，以18℃水为冷凝介质精馏分离乙醇碱溶液，至乙醇质量回收率超过96.2%，碱溶液中乙醇残余质量浓度低于0.03%，所得到的乙醇溶液、强碱性溶液即可回用。Add 300mL hemicellulose strong alkaline solution (pH 11.0, hemicellulose mass concentration 3.0%, sodium hydroxide mass concentration 17%) into the reaction tank, start the mechanical stirring device, add 300mL ethanol at a uniform speed until mixed, Stand at room temperature for 30 min until the precipitation is complete. Use a straw to absorb the supernatant A to 400mL, use a tube centrifuge to centrifuge the remaining solution under the condition of 5844g centrifugal force for 60min to obtain the precipitate, and wash it twice with 500mL ethanol solution (the initial volume ratio of ethanol and water is 80%:20%) 1. Centrifuge the sediment to obtain hemicellulose, and the recovery rate of hemicellulose reaches 91.4%; combine the centrifugal supernatant to obtain ethanol alkali solution, and the recovery rate of alkali reaches 95%. Use a rotary evaporator, control the vacuum degree of 100mbar and the temperature of the bottom liquid at 60~62°C, and use 18°C water as the condensing medium to rectify and separate the ethanol-alkali solution until the ethanol mass recovery rate exceeds 96.2%, and the residual mass concentration of ethanol in the alkali solution If it is less than 0.03%, the obtained ethanol solution and strong alkaline solution can be reused.
对比例2Comparative example 2
在锥底不锈钢反应罐中加入10L半纤维素强碱性溶液（pH13.8，半纤维素质量浓度4.0%，氢氧化钠质量浓度20%），启动机械搅拌装置，匀速流加8L乙醇至混合均匀，在室温条件下静置20min至沉淀完全。以虹吸管吸取上清液A至12~12.5L，采用管式离心机于5844g离心力条件下离心分离剩余溶液10min得到沉淀物，以2L乙醇溶液（乙醇与水初始体积比80%:20%）分两次洗涤、离心沉淀物得半纤维素，半纤维素回收率达92.6%；合并离心上清液得乙醇碱溶液，碱回收率达到98%。采用填料精馏塔，控制真空度100mbar和釜底料液温度68~70℃，以18℃水为冷凝介质精馏分离乙醇碱溶液，至乙醇质量回收率超过95%，碱溶液中乙醇残余质量浓度低于0.04%，所得到的乙醇溶液、强碱性溶液即可回用。Add 10L hemicellulose strong alkaline solution (pH13.8, hemicellulose mass concentration 4.0%, sodium hydroxide mass concentration 20%) into the conical bottom stainless steel reaction tank, start the mechanical stirring device, and add 8L ethanol at a constant speed until mixed Evenly, let it stand at room temperature for 20 minutes until the precipitation is complete. Use a siphon to absorb the supernatant A to 12~12.5L, use a tubular centrifuge to centrifuge the remaining solution for 10min under the condition of 5844g centrifugal force to obtain the precipitate, and divide it with 2L ethanol solution (the initial volume ratio of ethanol to water is 80%:20%) Wash twice and centrifuge the precipitate to get hemicellulose, the hemicellulose recovery rate reaches 92.6%; combine the centrifuged supernatants to get ethanol alkali solution, the alkali recovery rate reaches 98%. A packed rectification tower is used to control the vacuum degree of 100mbar and the temperature of the liquid at the bottom of the tank to be 68~70°C. Water at 18°C is used as the condensing medium to rectify and separate the ethanol-alkali solution until the recovery rate of ethanol exceeds 95%, and the residual mass of ethanol in the alkali solution If the concentration is lower than 0.04%, the obtained ethanol solution and strong alkaline solution can be reused.
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