WO2013131225A1 - 一种桉木片水解液生产木糖醇的方法及水解塔 - Google Patents

一种桉木片水解液生产木糖醇的方法及水解塔 Download PDF

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Publication number
WO2013131225A1
WO2013131225A1 PCT/CN2012/001748 CN2012001748W WO2013131225A1 WO 2013131225 A1 WO2013131225 A1 WO 2013131225A1 CN 2012001748 W CN2012001748 W CN 2012001748W WO 2013131225 A1 WO2013131225 A1 WO 2013131225A1
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Prior art keywords
hydrolysis
eucalyptus
tower
hydrolyzate
hydrolysate
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PCT/CN2012/001748
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English (en)
French (fr)
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应广东
陈克复
刘泽华
刘延波
乔军
张伟
翟丙彦
梁洪金
路庆辉
钟洪霞
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山东太阳纸业股份有限公司
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Priority to AU2012372733A priority Critical patent/AU2012372733B2/en
Priority to KR1020147025205A priority patent/KR101586620B1/ko
Publication of WO2013131225A1 publication Critical patent/WO2013131225A1/zh

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    • 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

Definitions

  • the present invention relates to a method for producing xylitol, and more particularly to a method for producing xylitol by pre-extracting hydrolyzate of eucalyptus dissolving pulp, and to a hydrolysis tower used in the hydrolysis. Background technique
  • Xylitol is an important chemical raw material and a sweet substance with nutritional value. It can be used to prepare surfactants, emulsifiers, demulsifiers, alkyds and coatings. It is a raw material for the manufacture of various drugs in the pharmaceutical industry. It is suitable for the health needs of human body. It also has good process characteristics and sensory characteristics suitable for making sugar-free candy. Especially food-grade xylitol has gradually entered people's life with its unique advantages and has broad market prospects.
  • domestic xylitol production mainly uses corn cob as raw material, which is decomposed into xylose liquid after acid hydrolysis, purified by decolorization and ion exchange resin, crystallized and separated to obtain xylose, and crystallized xylose is hydrogenated in the presence of catalyst. Prepare xylitol.
  • the production process using corncob as raw material mainly has the following shortcomings:
  • the corncob is used as a raw material to produce xylitol, and the utilization value of the waste residue is low;
  • the corn cob has many impurities and high ash content. It needs to be pretreated with water washing, acid boiling and boiling.
  • the batch hydrolysis process requires complex processes such as potting, acid addition, hydrolysis, extraction, and unloading, and the production efficiency is low.
  • Elm is a resource-rich renewable resource, and pulp and paper consumes a lot every year.
  • hemicellulose 20%-25% hemicellulose is mixed with the pulp black liquor in the form of wood chip hydrolysate and burned into the alkali recovery system.
  • the heat value of hemicellulose is only half of the lignin, and it is easy to scale when concentrated and burned. , causing waste of resources and energy. Summary of the invention
  • the present invention provides a method for producing xylitol from a eucalyptus hydrolysate, which is characterized by: using a hardwood eucalyptus as a raw material, using a continuous acid-free hydrolysis process, in a hydrolysis tower Pre-hydrolysis of eucalyptus chips saves time and improves production efficiency;
  • a hydrolysis tower is designed to continuously pre-hydrolyze the wood chips, which overcomes the complicated processes such as filling, acidizing, hydrolyzing, extracting and unloading in the batch hydrolysis process, thereby improving production. effectiveness.
  • the invention relates to a method for pre-extracting hydrolyzate of eucalyptus dissolving pulp to produce xylitol, comprising the following steps: pre-hydrolysis of eucalyptus chips, acid hydrolysis of pre-hydrolyzed hydrolyzate, decolorization of hydrolyzate, ion exchange purification, Concentrated and crystallized to obtain xylose, and then xylose is dissolved, hydrogenated, decolorized and purified, and crystallized to obtain xylitol.
  • the method is characterized in that pre-hydrolysis of eucalyptus chips is carried out in a hydrolysis tower, after pre-hydrolysis, The hydrolyzate is extracted from the hydrolysis tower, and the hydrolyzate is subjected to acid hydrolysis.
  • the reaction conditions are: pre-hydrolysis time l_4h, pre-hydrolysis temperature 120-180 ° C, pressure 0. 5- 0. 8Mpa, ratio of material to liquid 1: 3 - 10, wherein The material is eucalyptus, and the liquid is water.
  • the above-mentioned eucalyptus tablets are subjected to acid hydrolysis by the hydrolyzate obtained by pre-hydrolysis, and the reaction conditions for acid hydrolysis are: lyophilized solution dry matter concentration: 5%-15%, sulfuric acid concentration: 5-20 g/l, temperature: 100- 130°C, time: 60-140min o
  • the hydrolysis tower used in the above method, the hydrolysis tower comprises a tower body, the upper part of the tower body has a feed inlet, the bottom of the tower body has a discharge port, the lower part of the tower body has an extraction port with a filtering device, and the top of the tower has a steam inlet. .
  • the upper part of the tower body has a screw feeding mechanism, and the screw feeding mechanism comprises a double-layer screen, a bottom plate fixedly connected with the double-layer screen, and a spiral conveying shaft located above the bottom plate, wherein the inner layer of the double-layer screen is a screen.
  • the outer layer is a baffle layer, the baffle layer is fixed outside the screen, and there is a gap between the screen and the baffle layer; the lower part of the double-layer screen has a feed port and a circulating water outlet.
  • the filtering device at the extraction port is a sieve plate corresponding to the extraction port on the inner wall of the column.
  • the horizontal position of the dilution nozzle is located between the discharge port and the extraction port.
  • the acid-free continuous hydrolysis of eucalyptus reduces the complex pretreatment process of raw materials such as water washing, acid boiling and boiling, and reduces the water and acid amount of pretreatment;
  • the hydrolyzed wood chips further produce dissolving pulp, which solves the problem of low utilization value of waste slag using corn cob and the like as raw materials; 4. Realizing the high value utilization of resources, improving the utilization rate of raw materials and reducing environmental pollution;
  • the prior art batch hydrolysis process requires complicated processes such as filling the pot, adding acid solution, hydrolyzing, extracting, discharging, etc., and the production efficiency is low. , saving time and improving efficiency.
  • Figure 1 is a schematic view showing the structure of a hydrolysis tower of the present invention
  • 1-tower 2-bottom; 3-screen; 4-screw conveyor shaft; 5-feed port; 6- circulating water outlet; 7-steam inlet; 8-screen filter plate; Port; 10-mixer; 11-outlet; 12-dilution nozzle, 13-stop layer.
  • the aqueous solution of eucalyptus chips is pumped into a continuous hydrolysis tower.
  • the hydrolysis time of eucalyptus chips is 2.5 h
  • the reaction temperature is 165° (:
  • the pressure is 0.7 MPa
  • the mass ratio of eucalyptus to water is 1:4, and the lower part of the reaction tower will be
  • the hydrolyzate was continuously extracted, and the conversion of pentose sugar reached 60.8%;
  • the eucalyptus hydrolysate was hydrolyzed at a concentration of 10 g/l of sulfuric acid and a temperature of 120 ° C for 90 min.
  • the dry matter concentration was 5%
  • the inorganic acid content was 1.2%
  • the xylose purity was 65%.
  • the hydrolyzate was decolorized for 40 min at a temperature of 75 ° C, and the amount of activated carbon added was 7% of the dry matter.
  • the decolorizing solution was ion-exchanged according to the Yin-Yang process to obtain an ion exchange. Liquid, shading: 5%, light transmission 86.5 ° /. Total acid: 0.4%;
  • the primary ion exchange solution is concentrated to 40% xylose content, and the acidity is further reduced and the impurity ions are removed according to the Yin-Yang-Yin ion exchange process to obtain a xylose purification liquid having a purity of 95. %, concentrated to 80%, crystallized, and separated xylose.
  • the xylose produced by crystallization is dissolved by 50%, and the hydrogenation process is carried out at a pressure of 6.5 MPa, a temperature of 120 ° C, a pH of 8.0, and a catalyst of 3%. After hydrogenation, decolorization, ion exchange purification, and concentration to a sugar mass fraction of 85% are carried out. Crystallization, separation of xylitol. The xylitol had a purity of 98.7%.
  • the hydrolysis tower used in the above-mentioned raw method the hydrolysis tower comprises a tower body 1, the upper part of the tower body 1 has a feed port 5, the bottom of the tower body has a discharge port 11, and the bottom of the tower body 1 has a suction port with a filtering device. 9.
  • the upper part of the tower body 1 has a screw feeding mechanism, which comprises a double-layer screen, a bottom plate 2 fixedly connected to the double-layer screen, and a spiral conveying shaft located above the bottom plate, and the inner layer of the double-layer screen
  • the outer layer is the baffle layer 13
  • the baffle layer 13 is fixed on the screen 3, and there is a gap between the screen 3 and the baffle layer 13
  • the lower part of the double-layer screen has a feed port 5 and circulating water outlet 6.
  • the filtering device at the extraction port 9 is a sieve plate 8 corresponding to the extraction opening 9 on the inner wall of the tower body 1.
  • the bottom of the tower body 1 has a stirrer 10 at the bottom.
  • the bottom of the tower body 1 has a dilution nozzle 12.
  • the horizontal position of the dilution port 12 is located between the discharge port 11 and the extraction port 9.
  • the aqueous solution of the eucalyptus When feeding, the aqueous solution of the eucalyptus is pumped into the continuous hydrolysis tower, the water of the eucalyptus The solution enters the screw feeding mechanism through the feeding port 5, and the screw conveying shaft is rotated by the motor, so that the aqueous solution of the eucalyptus piece continuously enters into the tower body 1, and the water filtered by the double-layer screen is discharged from the circulating water outlet, and is reused.
  • the wood chip aqueous solution entering the tower body 1 is pre-hydrolyzed by the heat supplied by the steam, and the hydrolyzed liquid after the pre-hydrolysis is extracted through the extraction port, the eucalyptus wood piece is discharged from the discharge port 11, and the agitator 10 located at the bottom of the tower body 1 is continuously
  • the material is stirred and diluted with water by the dilution port 12, so that the eucalyptus chips are smoothly discharged from the discharge port 11 to prevent the wood chips from forming a plug.
  • Example 2 The aqueous solution of eucalyptus chips was pumped into a continuous hydrolysis tower.
  • the hydrolysis time of the eucalyptus chips was 3 h, the reaction temperature was 170 ° C, the pressure was 0.76 MPa, and the mass ratio of eucalyptus chips to water was 1:4.
  • the lower part of the hydrolysate was continuously extracted, and the conversion of pentose sugar reached 63.3%.
  • the hydrolyzate of eucalyptus wood was hydrolyzed at a concentration of sulfuric acid, krypton and temperature of 120 °C for 120 min, and the dry matter concentration was 8%, and the inorganic acid content was 0.8.
  • the purity of xylose is 67.5%; the hydrolyzate is decolorized for 45 minutes, the temperature is 80 ° C, the amount of activated carbon is 10% of the dry matter, and the decolorizing solution is ion exchanged according to the Yin-Yang process to obtain an ion exchange solution.
  • the aqueous solution of the wood chips is pumped into the continuous hydrolysis tower, the hydrolysis reaction time of the wood chips is 4 h, the reaction temperature is 170 ° C, the pressure is 0.76%, the mass ratio of the wood chips to the water is 1:4, and the hydrolyzate is continuously pumped in the lower part of the reaction tower. It is proposed that the conversion rate of pentose sugar reaches 64.3%;
  • the eucalyptus hydrolyzate was hydrolyzed for 120 min at a sulfuric acid concentration of 8 g/l and a temperature of 120 ° C.
  • the dry matter concentration was 12%, the inorganic acid content was 1.0%, and the xylose purity was 69%.
  • the hydrolyzate was decolorized for 45 min, the temperature was 70 ° C, and the amount of activated carbon was 10% of the dry matter.
  • the decolorizing solution was ion-exchanged according to the Yin-Yang process to obtain an ion exchange solution, shading: 10%, light transmission 89 %, total acid: 0.4%;
  • the primary ion exchange liquid is concentrated to a xylose content of 55%, and the acidity and the impurity ions are further removed according to the Yin-Yang-Yin ion exchange process to obtain a xylose purification liquid having a purity of 97.5% and concentration to 85%. After crystallization, separation of xylose;
  • the xylose produced by crystallization is dissolved by 50%, and the hydrogenation process is carried out at a pressure of 6.0 MPa, a temperature of 110 ° C, a pH of 7.5, and a catalyst of 4%. After hydrogenation, decolorization, ion exchange purification, and concentration to a sugar mass fraction of 85% are carried out. Crystallization, separation of xylitol, its purity reached 99%.

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Abstract

公开了一种木糖醇的生产方法，具体涉及一种桉木溶解浆木片预抽提水解液生产木糖醇的方法，还涉及该水解过程中所用到的水解塔。一种桉木溶解浆木片预抽提水解液生产木糖醇的方法，包括下述的步骤：桉木片预水解，对预水解的水解液进行酸水解，再对水解液脱色、离子交换纯化、浓缩、结晶处理得木糖，再对木糖经过溶解、加氢、脱色纯化、结晶处理得木糖醇，其特征在于：所述的桉木片预水解是在水解塔中进行，预水解之后，将水解液由水解塔中抽提出来，再对水解液进行酸水解。由于连续进料，不断水解，从而减少了现有技术中间歇水解工艺需装锅、加酸液、水解、抽提、卸料等复杂的工序，生产效率低的问题，节省了时间，提高了效率。

Description

一种桉木片水解液生产木糖醇的方法及水解塔 技术领域
本发明涉及一种木糖醇的生产方法，具体涉及一种桉木溶解浆木 片预抽提水解液生产木糖醇的方法，还涉及该水解过程中所用到的水 解塔。 背景技术
木糖醇是一种重要的化工原料和具有营养价值的甜味物质，可制 取表面活性剂、 乳化剂、 破乳剂、 醇酸树脂及涂料， 是医药工业制造 各种药物的原料， 不仅具有适合人体健康需要的特性，还具有适于制 作无糖糖果的良好工艺特性和感官特性，尤其是食品级木糖醇以独特 的优势逐渐走进了人们的生活， 具有广阔的市场前景。
目前国内木糖醇生产主要以玉米芯为原料，经酸解后分解为木糖 液， 经脱色、 离子交换树脂净化提纯、 结晶、 分离制取木糖， 结晶木 糖再在催化剂存在下加氢制取木糖醇。
(C5H804)n+nH20 ^nC5H10O5
C5H10O5+ H2 _ ^ C5H1205
以玉米芯为原料的生产工艺主要存在以下不足：
1、 玉米芯等原料的季节性很明显， 需要大量的储存空间；
2、 玉米芯等为原料生产木糖醇， 废渣利用价值低；
3、 玉米芯中杂质多， 灰分含量高， 需进行水洗、 酸煮、 水煮等 预处理；
4、 间歇水解工艺需装锅、 加酸液、 水解、 抽提、 卸料等复杂的 工序， 生产效率低。
桉木是一种资源丰富的可再生资源，制浆造纸每年都要消耗大量
确认本 的桉木， 除纤维素以纸浆的形式被有效利用外， 占到质量分数
20%-25%的半纤维素以木片水解液形式与制浆黑液混合进入到碱回 收系统被烧掉， 半纤维素的热值仅仅是木质素的一半，浓縮燃烧时极 易结垢， 造成资源和能源浪费。 发明内容
针对现有技术的不足，本发明提供了一种桉木片水解液生产木糖 醇的方法， 该方法的特点是： 以阔叶木桉木为原料， 采用连续的无酸 水解工艺， 在水解塔中对桉木片进行预水解， 节约了时间， 提高了生 产效率；
本发明的另一个特点是， 设计了一种水解塔对按木片连续预水 解， 克服了间歇水解工艺中需要装锅、 加酸液、 水解、 抽提、 卸料等 复杂的工序， 提高了生产效率。
本发明的技术方案为：
一种桉木溶解浆木片预抽提水解液生产木糖醇的方法，包括下述 的步骤： 桉木片预水解， 对预水解的水解液进行酸水解， 再对水解液脱色、 离 子交换纯化、 浓缩、 结晶处理得木糖， 再对木糖经过溶解、 加氢、 脱 色纯化、 结晶处理得木糖醇， 该方法的特点是， 桉木片预水解是在水 解塔中进行， 预水解之后， 将水解液由水解塔中抽提出来， 再对水解 液进行酸水解。
上述的桉木片的预水解过程中，其反应条件为：预水解时间 l_4h, 预水解温度 120°C-180°C , 压力 0. 5- 0. 8Mpa， 料液比 1 : 3 — 10， 其 中料为桉木片， 液为水。 上述的桉木片经过预水解后的得到的水解液再进行酸水解，酸水解的 反应条件是： 水解液干物质浓度： 5%-15%， 硫酸浓度： 5-20g/l， 温 度： 100- 130°C， 时间： 60-140mino
上述的方法中用到的水解塔，该水解塔包括塔体，塔体上部有进料口、 塔体底部有出料口、塔体下部有带过滤装置的抽提口、塔顶有蒸汽入 口。
塔体内的上部有螺旋送料机构， 该螺旋送料机构包括双层筛网、与双 层筛网固定连接的底板和位于底板上方的螺旋输送轴，上述的双层筛 网的内层为筛网， 外层为挡料层， 挡料层固定在筛网外， 筛网与挡料 层之间有间隙； 上述的双层筛网的下部有进料口和循环水出口。
抽提口处的过滤装置为塔体内壁上与抽提口相对应的筛滤板。
塔体内的底部有搅拌器。
塔体底部有稀释水口。
稀释水口的水平位置位于出料口和抽提口之间。
本发明的有益效果是：
1、 桉木的无酸连续水解减少对原料的水洗、 酸煮、 水煮等复杂 的预处理工序， 减少了预处理的用水、 酸量；
2、 为木糖醇生产开辟了新的丰富的原料资源和方法， 解决玉米 芯等原料供应不稳定性的难题；
3、 水解后的木片进一步生产溶解浆， 解决了以玉米芯等为原料 的废渣利用价值低的难题； 4、 实现了资源高值化利用， 提高了原料利用率的同时也减轻了 环境污染；
5、 由于本发明的方法是连续进料， 不断水解， 从而减少了现有 技术中间歇水解工艺需装锅、 加酸液、 水解、 抽提、 卸料等复杂的工 序， 生产效率低的问题， 节省了时间， 提高了效率。
附图说明
图 1为本发明的水解塔的结构示意图；
图中， 1-塔体； 2-底板； 3-筛网； 4-螺旋输送轴； 5-进料口； 6- 循环水出口； 7-蒸汽入口； 8-筛滤板； 9-抽提口； 10-搅拌器； 11-出料 口； 12-稀释水口， 13-挡料层。
具体实施方式
下面结合具体实施例对本发明作更进一步的说明，以便本领域的 技术人员更了解本发明， 但并不因此限制本发明。
实施例 1
将桉木片的水溶液用泵打到连续水解塔中，桉木片水解反应时间 2.5h, 反应温度 165° (：， 压力 0.7MPa， 桉木片与水的质量比为 1:4， 在反应塔下部将水解液连续抽提出来， 戊糖转化率达到了 60.8%;
桉木片水解液在硫酸浓度 10g/l、温度 120°C条件下，水解 90min， 其干物质浓度为 5%， 无机酸含量 1.2%， 木糖纯度 65%;
将水解液脱色处理 40min，温度 75°C，加入活性炭的量为干物质 的 7%， 脱色液按照阴-阳工艺流程进行离子交换， 得到一次离子交换 液， 遮光： 5%、 透光 86.5°/。、 总酸： 0.4%; 将一次离子交换液浓缩至木糖含量 40%， 按照阴-阳 -阴的离子交 换工艺进一步降低酸度和除去其中的杂质离子， 得到木糖净化液， 其 纯度为 95%， 浓缩到 80%后进行结晶、 分离出木糖。 将结晶生产的木糖溶解 50%， 进行加氢工序， 压力 6.5MPa， 温 度 120°C， pH8.0， 催化剂 3%， 氢化后进行脱色、 离子交换纯化后浓 缩至糖质量分数 85%, 经结晶、 分离出木糖醇。 该木糖醇的纯度为 98.7%。 上述的生方法中用到的水解塔， 该水解塔包括塔体 1， 塔体 1上 部有进料口 5、塔体底部有出料口 11、塔体 1下部有带过滤装置的抽 提口 9、 塔顶有蒸汽入口 7。 塔体 1 内的上部有螺旋送料机构， 该螺旋送料机构包括双层筛 网、与双层筛网固定连接的底板 2和位于底板上方的螺旋输送轴， 所 述的双层筛网的内层为筛网， 外层为挡料层 13， 挡料层 13固定在筛 网 3夕卜， 筛网 3与挡料层 13之间有间隙； 所述的双层筛网的下部有 进料口 5和循环水出口 6。 抽提口 9处的过滤装置为塔体 1内壁上与抽提口 9相对应的筛滤 板 8。 塔体 1内的底部有搅拌器 10。 塔体 1底部有稀释水口 12。
稀释水口 12的水平位置位于出料口 11和抽提口 9之间。
进料时， 将桉木片的水溶液用泵泵入连续水解塔中， 桉木片的水 溶液通过进料口 5进入螺旋进料机构， 螺旋输送轴由电机带动旋转， 使桉木片的水溶液不断的进入到塔体 1内，双层筛网滤出的水由循环 水出口排出， 重复利用， 进入塔体 1内的木片水溶液由蒸汽提供热量 进行预水解， 预水解后的水解液通过抽提口抽提出， 桉木片由出料口 11排出， 位于塔体 1底部的搅拌器 10不断的对物料进行搅拌， 同时 通过稀释口 12加水稀释， 实现桉木片由出料口 11顺利排出， 防止木 片形成料塞。 实施例 2 将桉木片的水溶液用泵打到连续水解塔中，桉木片水解反应时间 3h， 反应温度 170°C， 压力为 0.76MPa， 桉木片与水的质量比为 1:4， 在反应塔下部将水解液连续抽提出来， 戊糖转化率达到了 63.3%; 桉木片水解液在硫酸浓度，≠、温度 120 °C条件下，水解 120min， 其干物质浓度为 8%， 无机酸含量 0.8%， 木糖纯度 67.5%; 将水解液进行脱色处理 45min，温度 80°C，加入活性炭的量为干 物质的 10%， 脱色液按照阴-阳工艺流程进行离子交换， 得到一次离 子交换液， 遮光： 8%、 透光 89%、 总酸： 0.3%; 将一次离子交换液浓缩至木糖含量 50%， 按照阴-阳 -阴的离子交 换工艺进一步降低酸度和除去其中的杂质离子， 得到木糖净化液， 其 纯度为 97%， 浓縮到 80%后进行结晶、 分离出木糖； 将结晶生产的木糖溶解 50%， 进行加氢工序， 压力 6.0MPa， 温 度 110°C， pH7.5, 催化剂 3%， 氢化后进行脱色、 离子交换纯化后浓 缩至糖质量分数 85%， 经结晶、 分离出木糖醇， 纯度为 98.9%。 实施例 3
将木片的水溶液用泵打到连续水解塔中， 木片水解反应时间 4h， 反应温度 170°C， 压力为 0.76%， 木片与水的质量比为 1:4， 在反应塔 下部将水解液连续抽提出来， 戊糖转化率达到了 64.3%;
桉木水解液在硫酸浓度 8g/l、 温度 120°C条件下， 水解 120min， 其干物质浓度为 12%， 无机酸含量 1.0%， 木糖纯度 69%;
将水解液进行脱色处理 45min，温度 70°C，加入活性炭的量为干 物质的 10%， 脱色液按照阴-阳工艺流程进行离子交换， 得到一次离 子交换液， 遮光： 10%、 透光 89%、 总酸: 0.4%;
将一次离子交换液浓縮至木糖含量 55%， 按照阴-阳 -阴的离子交 换工艺进一步降低酸度和除去其中的杂质离子， 得到木糖净化液， 其 纯度为 97.5%， 浓缩到 85%后进行结晶、 分离出木糖；
将结晶生产的木糖溶解 50%， 进行加氢工序， 压力 6.0MPa， 温 度 110°C， pH7.5, 催化剂 4%， 氢化后进行脱色、 离子交换纯化后浓 缩至糖质量分数 85%, 经结晶、 分离出木糖醇， 其纯度达到 99%。

Claims

权利要求
1. 一种桉木溶解浆木片预抽提水解液生产木糖醇的方法， 包括 下述的步骤：
桉木片预水解， 对预水解的水解液进行酸水解， 再对水解液脱色、 离 子交换纯化、 浓缩、 结晶处理得木糖， 再对木糖经过溶解、 加氢、 脱 色纯化、 结晶处理得木糖醇， 其特征在于： 所述的桉木片预水解在水 解塔中进行， 预水解之后， 将水解液由水解塔中抽提出来， 再对水解 液进行酸水解。
2. 如权利要求 1所述的一种桉木溶解桨木片预抽提水解液生产 木糖醇的方法， 其特征在于： 所述的桉木片的预水解过程中， 其反应 条件为：预水解时间 1- 4h，预水解温度 120°C-180°C，料液比 1 : 3 — 10， 压力 0. 5- 0. 8Mpa。
3. 如权利要求 1所述的一种桉木溶解浆木片预抽提水解液生产 木糖醇的方法，其特征在于：所述的桉木片预水解后的水解液酸水解， 其反应条件是： 水解液干物质浓度： 5%-15%， 硫酸浓度： 5- 20g/l， 温度： 100-130°C， 时间： 60- 140min。
4. 一种如权利要求 3 所述的生方法中用到的水解塔， 其特征在 于， 该水解塔包括塔体， 所述的塔体上部有进料口、塔体底部有出料 口、 塔体下部有带过滤装置的抽提口、 塔顶有蒸汽入口。
5. 如权利要求 4所述的一种水解塔， 其特征在于， 所述塔体内 的上部有螺旋送料机构， 所述的螺旋送料机构包括双层筛网、与双层 筛网固定连接的底板和位于底板上方的螺旋输送轴，所述的双层筛网 的内层为筛网， 外层为挡料层， 挡料层固定在筛网外， 筛网与挡料层 之间有间隙； 所述的双层筛网的下部有进料口和循环水出口。
6. 如权利要求 5所述的一种水解塔， 其特征在于， 所述的抽提 口处的过滤装置为塔体内壁上与抽提口相对应的筛滤板。
7. 如权利要求 6所述的一种水解塔， 其特征在于， 所述的塔体 内的底部有搅拌器。
8. 如权利要求 7所述的一种水解塔， 其特征在于， 所述的塔体 底部有稀释水口。
9. 如权利要求 8所述的一种水解塔， 其特征在于， 所述的稀释 水口的水平位置位于出料口和抽提口之间。
PCT/CN2012/001748 2012-03-08 2012-12-28 一种桉木片水解液生产木糖醇的方法及水解塔 WO2013131225A1 (zh)

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