CN105669419B - The method of sequential simulated moving bed separation corn stalk acidolysis liquid sugar acids - Google Patents

The method of sequential simulated moving bed separation corn stalk acidolysis liquid sugar acids Download PDF

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CN105669419B
CN105669419B CN 201610010820 CN201610010820A CN105669419B CN 105669419 B CN105669419 B CN 105669419B CN 201610010820 CN201610010820 CN 201610010820 CN 201610010820 A CN201610010820 A CN 201610010820A CN 105669419 B CN105669419 B CN 105669419B
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sulfuric acid
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sugar
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CN105669419A (en )
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曹龙奎
李洪飞
李文杰
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黑龙江八农垦大学
黑龙江八一农垦大学
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本发明涉及的是顺序式模拟移动床分离玉米秸秆酸解液中糖酸的方法,它具体为:将玉米秸秆酸解液通过顺序式模拟移动床色谱设备分离,分离阶段,8根色谱柱串联,由第3柱下的循环泵将柱中液体抽出注入第4根柱,第4根柱中液体注入第5根柱中,依次循环操作;解吸阶段,在第1根柱上部进入解吸剂,第6根柱下放出硫酸溶液;进料解吸阶段,在第1根柱上部进入解吸剂,第5根色谱柱上部进入所述玉米秸秆酸解液,第1根柱下放出糖溶液,第6根色谱柱下放出硫酸溶液;分离得到的硫酸溶液浓度为210mg/mL~320mg/mL,糖溶液浓度为20mg/mL~41mg/mL;硫酸溶液浓缩回收;糖溶液过滤浓缩。 The present invention relates to a method in corn stover acid hydrolyzate sugar acids sequential simulated moving bed separation, it is specifically: Corn stover hydrolyzate acid by sequential simulated moving bed chromatographic separation device, the separation stage, eight columns in series , by the circulation pump in the third column to column injection of a liquid withdrawn four column, four column of the liquid injection 5 Genzhu sequentially circulating operation; desorption phase, the first desorbent into the upper portion of pillars, 6 Genzhu discharged under a sulfuric acid solution; desorption stage feed, enter the upper portion of pillars of the first desorbent, the column into the upper portion 5 of the corn stover acid hydrolyzate, sugar solution discharged under Genzhu first and 6 sulfuric acid solution discharged root column; sulfuric acid concentration of the solution obtained was isolated 210mg / mL ~ 320mg / mL, concentration of the sugar solution of 20mg / mL ~ 41mg / mL; solution was concentrated recovered sulfuric acid; a sugar solution was filtered and concentrated. 本发明分离后的硫酸浓度高,糖溶液浓度高,解决了玉米秸秆再利用中硫酸回收难题,成本低。 High concentration of sulfuric acid after the separation of the present invention, high concentration sugar solutions, corn stalk solve recovery problems reuse of sulfuric acid, and low cost.

Description

顺序式模拟移动床分离玉米秸秆酸解液中糖酸的方法 The method of sequential simulated moving bed separation corn stalk acidolysis liquid sugar acids

[0001] 一、技术领域 [0001] I. Field

[0002] 本发明涉及的是玉米秸杆酸解液中硫酸和糖液的分离技术,具体涉及顺序式模拟移动床分离玉米秸秆酸解液中糖酸的方法。 [0002] The present invention relates to corn stover sulfuric acid solution and sugar mixture separation technology, particularly relates to a method of sequential simulated moving bed separation corn stalk acidolysis liquid sugar acids. _] 二、背景技术 _] II. Background

[0004]我国是一个农业大国,各类农作物纤维资源十分丰富,仅秸秆一项每年就达7亿吨以上,其中玉米秸秆约2.2亿吨。 [0004] Our country is a large agricultural country, all kinds of fiber crops very rich in resources, it is only a straw up to 7 million tons per year, of which about 220 million tons of corn stover. 但目前除一小部分用作反刍动物的饲料外,其余部分多以燃料烧掉,造成大气严重污染。 But in addition to a small fraction as feed for ruminants, the remaining portion of the plurality of fuel to burn, causing atmospheric pollution. 玉米秸杆中含有大量的纤维素和半纤维素,可通过多种途径转化成糖,作为发酵工业低成本原料的来源。 Corn stover contains large amounts of cellulose and hemicellulose can be converted into sugars by various routes, fermentation industry as a source of low cost raw materials.

[0005] 玉米秸秆制糖以硫酸水解法和酶降解法为主,其中,因酶类成本高,生产效率低, 所以酶降解法未大规模用于玉米秸杆的水解应用。 [0005] The corn stalk sugar sulfuric acid hydrolysis and enzymatic degradation mainly, wherein the enzyme due to high costs, low productivity, the enzyme degradation is not large-scale applications for the hydrolysis of corn stover. 硫酸水解玉米秸秆在工艺流程、生产成本和总糖收率上都具有明显优势,可大规模应用于玉米秸杆的预处理。 Sulfuric acid hydrolysis process in the corn stalks, sugar yields and total production cost has obvious advantages, it can be widely applied in the pretreatment of corn stover. 但该方法中硫酸的去除一直是困扰企业生存和发展的难题,利用离子交换树脂法对玉米秸秆水解液中的硫酸进行吸附,存在成本高、效率低的问题,同时再生离子交换树脂的冲洗液排放会造成大量的污染。 However, removal of this method sulfuric acid has been troubled by the survival and development problems, the use of ion exchange resin of corn stover hydrolyzate sulfate adsorption, high cost, low efficiency problems, while reproducing the rinse liquid ion exchange resin emissions will cause a lot of pollution. 因此,有效的将玉米秸秆酸解液中的硫酸进行回收,并控制其回收成本,同时将玉米秸杆酸解液进行高附加值的利用是玉米秸杆再利用中的主要研宄内容。 Thus, effective solutions of corn stover liquid sulfuric acid recovery, and controlling the recovery cost, while corn stover was subjected to acid hydrolysis with a high value-added content is the main study based on straw reuse maize.

[0006]中国专利2〇12100〇5679.4公开一种木质纤维素水解物的糖、酸、盐分离方法,文中提及利用模拟移动床对水解液进行糖酸分离,分离时无机酸、盐为快组分,糖、醋酸为慢组分,并没有将醋酸与糖完全分开,且没有列出具体的模拟移动床分离工艺及条件。 [0006] Chinese Patent 2〇12100〇5679.4 discloses a lignocellulosic hydrolyzate sugars, organic acids, salts of separation methods, references to the use of simulated moving bed separation saccharic acid was subjected to hydrolysis, separation of inorganic acids, salts faster component, a sugar, acetic acid as the slow component, does not completely separate the acetic acid and sugar, and in particular of a simulated moving bed separation processes and conditions were not listed.

[0007]李潯等报道了模拟移动床离子排斥色谱分离水解液中的糖酸的研究[太阳能学报,2005,29⑹:747_751],其主要内容为利用8柱4区连续模拟移动床对生物质水解液进行糖酸分离,原料中硫酸的浓度是12%〜15%,提取液中糖浓度为1 • 5%〜2 • 0%,采用的模拟移动床分离工艺为传统4区模式,该模式是连续进料、连续洗脱,作用于物质分离的时间较短,存在生产效率低,溶液回收成本高等问题。 [0007] Lee et al reported Au simulated moving bed ion exclusion chromatography study hydrolyzate sugar acids [SOLAR, 2005,29⑹: 747_751], whose main content is 8 column using a continuous simulated moving bed region 4 biomass saccharic acid hydrolysis liquid was separated, sulfuric acid concentration in the feed is 12% ~ 15%, the concentration of sugar extract 1 • 5% ~2 • 0%, simulated moving bed separation process using the traditional four zone mode, which a continuous feed, continuous elution, the separation of a substance acting short time, the presence of low productivity, high cost recovery solution. 由于这种限制,原料中干物质量很难提高,若提高会导致分离后产品纯度和收率下降。 Because of this limitation, the raw material is difficult to increase the amount of dry matter, if the increase will lead to isolation of the product purity and yield decrease.

[0008] 三、发明内容 [0008] III. SUMMARY OF THE INVENTION

[0009] 本发明目的i提供了顺序式模拟移动床分离玉米秸秆酸解液中糖酸的方法,这种顺序式模拟移动床分离玉米秸秆酸解液中糖酸的方法适用于解决传统模拟移动床分离工艺进行糖酸分离存在的溶液回收成本高、生产效率低的问题。 [0009] i object of the present invention provides a sequential simulated moving bed process corn stover acid hydrolyzate separated in sugar acids, such sequential simulated moving bed separation corn stover acid hydrolyzate sugar acid method is applicable to solve the conventional simulated moving bed separation process for high-cost sugar solution was recovered acid separation occurring, low production efficiency.

[0010] 为了实现上述目的,本发明采用的具体技术方案如下:这种顺序式模拟移动床分离玉米f秆酸解液中糖酸的方法,以玉米秸秆酸解液为原料,采用顺序式模拟移动床分离设备分离硫酸和糖液,玉米秸秆酸解液中硫酸含量500mg/ml〜700mg/ml、糖液含量60mg/ml 〜80mg/ml;具体如下: [0010] To achieve the above object, the present invention employs the specific technical solutions as follows: f in corn stalk acidolysis liquid sugar acids such sequential simulated moving bed separation, corn stover hydrolyzate acid as raw materials, sequential analog moving bed separation apparatus for separating sulfuric acid and sugar, corn stover hydrolyzate content of sulfuric acid 500mg / ml~700mg / ml, sugar content 60mg / ml ~80mg / ml; as follows:

[0011]_ ^顺序?模拟移动床分离:将所述玉米秸秆酸解液通过顺序式模拟移动床色谱设备进行分离,分离过程一个周期包括8步,每个步骤包括三个阶段,第一阶段为分离阶段,8 根色谱柱串联连接,由安装在第3柱下的循环泵将柱中液体抽出注入第4根柱,第4根柱中液体注入第5根柱中,依次往复进行循环操作;第二阶段为解吸阶段,在第i根柱上部进入解吸剂,第6根柱下放出硫酸溶液;第三阶段为进料解吸阶段,在第1根柱上部进入解吸剂,第5根色谱柱上部进入所述玉米秸杆酸解液,第1根柱下放出糖溶液,第6根色谱柱下放出硫酸溶液。 ? [0011] _ ^ sequential simulated moving bed separation: the acid hydrolysis of corn stover was isolated by sequential chromatographic simulated moving bed apparatus, a separation cycle comprising 8 steps, each step comprising three stages, the first stage as a separate phase, eight columns are connected in series, a circulation pump is mounted in the third column of the column of liquid withdrawn four column injection, the liquid injection four column 5 Genzhu sequentially reciprocated cycle of operation ; second stage desorption stage, the upper portion of the desorbent into the i-th Genzhu, the sulfuric acid solution discharged under 6 Genzhu; third stage is fed desorption phase, in the upper portion of pillars into the first desorbent, the first five chromatography portion of the column into the corn stover acid hydrolyzate, sugar solution discharged under Genzhu first, the sulfuric acid solution discharged under six columns. 这三个阶段完成后,解吸阶段和进料解吸阶段的进料口和出料口都依次向后移动一个色谱柱,再重复进行每个步骤的三个阶段,8步完成即8根色谱柱轮换一周即一个周期结束, 接下来进入下一个周期,方法与第一个周期相同,依次循环,直到分离过程达到稳态。 After completion of the three stages, desorption stage and desorption stage feed inlet and outfeed sequentially moved backward to a column, and then repeated three stages each step, i.e., the completion of step 8 8 column i.e. the end of a one week period of rotation, then the next cycle, in the same manner as the first cycle, in cycles, until a separation process reached a steady state. 分离得到的硫酸溶液浓度为210mg/mL〜320mg/mL、纯度为93%〜98%,糖溶液浓度为20mg/mL〜 41mg/mL、纯度93% 〜96%; A sulfuric acid concentration solution obtained was isolated 210mg / mL~320mg / mL, purity of 93% ~98% sugar solution at a concentration of 20mg / mL~ 41mg / mL, purity of 93% ~96%;

[0012] b、硫酸溶液浓缩回收:将经a步骤得到的硫酸溶液进行旋转蒸发处理,温度50°C〜 65 °C,得到浓缩液,浓缩液浓度为500mg/mL〜550mg/mL; [0012] b, and concentrated sulfuric acid solution recovered: a rotary evaporator will be treated with a sulfuric acid solution obtained in step, a temperature of 50 ° C~ 65 ° C, to obtain a concentrate, the concentrate at a concentration of 500mg / mL~550mg / mL;

[0013] c、糖溶液过滤:将a步骤制得糖溶液用微米级滤器进行过滤,制得澄清的黄色液体; [0013] c, sugar solution filtered: The step to prepare a sugar solution was filtered through a micron filter, to obtain a clear yellow liquid;

[0014] d、糖溶液浓缩:将C步骤制得糖溶液进行旋转蒸发处理,温度为60〜65°C,制得澄清的黄色液体。 [0014] d, concentrated sugar solution: The sugar solution obtained in step C by rotary evaporation process, the temperature is 60~65 ° C, to obtain a clear yellow liquid.

[0015] 上述方案中玉米秸秆酸解液的制备方法: [0015] Solutions were prepared of the above-described embodiment corn stover acid:

[0016] 第一步、玉米秸秆酸解液的制备:将玉米秸秆烘千、粉碎过40目筛,称取一定质量玉米秸秆,按照料液比1:50的比例添加体积浓度3%的硫酸溶液,置于微波萃取仪中,调整微波功率700W,温度80°C,反应153min,得到玉米秸秆酸解液; [0016] The first step, preparation of corn stover hydrolyzate acid: one thousand bake corn stover, sifted through a 40 mesh screen, weighed certain quality corn stover was added concentration of 3% by volume of sulfuric acid in accordance with the ratio of 1:50 stock solution solution was placed in a microwave extraction device, adjusting the microwave power 700W, a temperature of 80 ° C, the reaction 153min, corn stover acid hydrolyzate obtained;

[0017]第二步、用滤纸将第一步制得的玉米秸秆酸解液过滤,得到澄清深棕色液体,并利用旋转蒸发仪将其浓缩至溶液中硫酸含量500mg/ml〜700mg/ml、糖液含量60mg/ml〜80mg/ ml〇 [0017] The second step, with the filter paper was first step in acid hydrolysis of corn stover obtained was filtered to give a clear dark brown liquid, using a rotary evaporator and concentrated to a sulfuric acid content of the solution 500mg / ml~700mg / ml, sugar content of 60mg / ml~80mg / ml〇

[0018] 上述方案中步骤b得到的硫酸浓缩液稀释得到体积浓度3%的硫酸溶液,重复用于玉米秸杆酸解液制备的第一步中。 Dilution of the concentrated sulfuric acid solution in step [0018] b obtained above solution to give a concentration of 3 vol% sulfuric acid solution, prepared in the first step is repeated for corn stover acid hydrolyzate.

[0019] 上述方案中顺序式模拟移动床的分离中,吸附剂为阳离子交换树脂UBK08、IR120H +、IR118H+、IR120Na+或AMBERJET C1H+中的任何一种;解吸剂为去离子水,分离温度为5(TC 〜55°C,第一阶段循环量为410〜550mL;第二阶段,解吸剂流量为23〜45mL/min,解吸时间为110〜160s;第三阶段,解吸剂流量为30〜45mL/min,进料量为35〜50mL/min,进料和解吸时间为120〜180s。 [0019] separating said aspect sequential simulated moving bed, the adsorbent is a cation exchange resin UBK08, any IR120H +, IR118H +, IR120Na + or AMBERJET C1H + are; desorbent deionized water, separation temperature is 5 ( TC ~55 ° C, an amount of the first phase of the cycle 410~550mL; a second phase, the desorbent flow 23~45mL / min, desorption time 110~160s; the third phase, the desorbent flow 30~45mL / min , the feeding amount was 35~50mL / min, feed and desorption time 120~180s.

[0020] 有益效果: [0020] beneficial effects:

[0021] 1、本发明的核心技术为顺序式模拟移动床分离玉米秸杆酸解液中硫酸和糖液技术,以较高分离度将硫酸与糖液分离,所用原料硫酸浓度达到50%〜80%,糖液浓度为6%〜 8%,较李浔等所用生物质原料中的硫酸浓度高出3〜5倍,工艺的处理量明显增大;李浔等按照其报道的工艺[太阳能学报,2005,29 (6) :747_751]得到分离后的硫酸浓度最高为7%,糖液浓度最高为2%,硫酸和糖液纯度及收率达到93%。 [0021] 1, the core technology of the present invention is a sequential simulated moving bed separation corn stover hydrolyzate sulfuric acid and sugar technology, higher resolution and sulfuric acid sugar separation, the feed sulfuric acid concentration of ~ 50% 80%, sugar concentration of 6% to 8%, more Li Xun like biomass feedstock in a sulfuric acid concentration of 3 to 5 times higher with, the processing amount of the process significantly increased; Li et SBS process according to its reported [solar Technology, 2005,29 (6): 747_751] obtained after separation of sulfuric acid concentration up to 7% sugar concentration up to 2%, sulfuric acid and sugar purity and yield of 93%. 本发明工艺作用于物质分离的时间较长,分离后的硫酸浓度最高为31.8%、纯度可达97.8%,收率可达98%,糖溶液浓度最高为4 • 〇5%、纯度可达95%,收率可达97%;因此,本工艺在后续浓缩处理中会节省大量能源,且硫酸和糖液的收率及纯度较高,解决了玉米秸杆再利用中硫酸的回收难题,具有工序步骤简便,工艺成本节约等鲜明的特色。 Process of the present invention to effect separation of substances longer, after the separation of sulfuric acid concentration up to 31.8%, purity 97.8%, yield of 98% sugar solution up to a concentration of 4 • 〇5%, purity 95 %, yield 97%; Accordingly, the present process in the subsequent concentration treatment will save a lot of energy, and sulfuric acid, and high sugar yield and purity, to solve the problem of recovering corn stover reuse of sulfuric acid, having simple process steps, process cost savings, and other distinctive features.

[0022] 2、本发明采用顺序式模拟移动床对玉米秸杆酸解液中硫酸和糖液进行分离,得到硫酸溶液的收率为93%〜98%,糖溶液收率为94%〜97%。 [0022] 2, the present invention employs a sequential simulated moving bed of corn stover sulfuric acid hydrolysis and sugar was separated to obtain a solution of sulfuric acid in a yield of 93% ~98%, yield of 94% sugar solution ~97 %. 分离效果好,收率高,易于工业化生产放大。 Separation is good, high yield, easy industrial production enlarged.

[0023]四、具体实施方式 [0023] IV DETAILED DESCRIPTION

[0024]下面对本发明做进一步的说明: [0024] The following further illustrate the present invention:

[0025] 实施例1: [0025] Example 1:

[0026]这种顺序式模拟移动床分离玉米秸秆酸解液中糖酸的方法如下: [0026] The method of acid hydrolysis of corn stalk liquid sugar acids such sequential simulated moving bed separation as follows:

[0027] a、玉米秸秆酸解液的制备:将玉米秸秆烘干、粉碎过4〇目筛,称取2g玉米秸秆粉, 加入体积浓度3%的硫酸溶液1〇〇此,置于微波萃取伩中,调整微波功率700ff,温度8(rC,反应153min,得到玉米秸杆酸解液。 [0027] a, Preparation of corn stover hydrolyzate acid: corn stover dried, crushed 4〇 mesh sieve, corn stalk powder weighed 2g, was added sulfuric acid concentration of 3% by volume 1〇〇 this solution, placed in a microwave extraction Xin, adjusting the microwave power 700ff, temperature 8 (rC, the reaction 153min, to give an acid hydrolyzate of corn stover.

[0028] b、用滤纸将a步骤制得的玉米秸秆酸解液过滤,得到澄清深棕色液体,并利用旋转蒸发仪将其浓缩至溶液中硫酸浓度519 • 4mg/mL、糖液浓度61.49mg/mL。 [0028] b, the step of using a filter paper made of corn stover acid solution was filtered to give a clear dark brown liquid, using a rotary evaporator and concentrated to a sulfuric acid concentration in the solution 519 • 4mg / mL, sugar concentration 61.49mg / mL.

[0029] —cjf序式模拟移动床分离:处理后的玉米秸秆酸解液通过顺序式模拟移动床色谱设备进行分离,吸附剂为阳离子交换树脂UBK08;解吸剂为去离子水,分离温度为50。 [0029] -cjf frame sequential simulated moving bed separation: acid hydrolysis of corn stover was treated isolated by sequential simulated moving bed chromatographic apparatus, the adsorbent is a cation exchange resin UBK08; desorbent deionized water, separation temperature of 50 . (:,分离过程一个周期包括8步,每个步骤包括三个阶段,第一阶段为分离阶段,8根色谱柱串联连接,由安装在第3柱下的循环泵将柱中液体抽出注入第4根柱,第4根柱中液体注入第5根柱中,依次往复进行循环操作,循环量为410mL;第二阶段为解吸阶段,在第1根柱上部进入解吸剂,第6根柱下放出硫酸溶液,解吸剂流量为23.5mL/min,解吸时间为112s;第三阶段为进料解吸阶段,在第1根柱上部进入解吸剂,第5根色谱柱上部进入b步骤所得玉米秸秆酸解液^第1根柱下放出糖溶液,弟6根色谱柱下放出硫酸溶液,解吸剂流量为3 〇• 5 m L /min,进料量为42_2mL/min,进料和解吸时间为wos。这三个阶段完成后,解吸阶段和进料解吸阶段的进料口和出料口都依次向后移动一个色谱柱,再重复进行每个步骤的三个阶段,8步完成即8根色谱柱轮换二周即一个周期结束,接下来进入 (:, The separation process comprises a cycle of eight steps, each step comprising three stages, the first stage is a separation stage, eight columns are connected in series, a circulation pump is mounted in the third column of the column of liquid withdrawn injection four column, four column of the liquid injection 5 Genzhu sequentially reciprocated cycle of operation, the circulating volume of 410 mL; the second stage desorption stage, the upper portion of pillars into the first desorbent, the sixth Genzhu sulfuric acid solution discharged, the desorbent flow rate of 23.5mL / min, desorption time is 112S; the third stage of the desorption stage feed, enter the upper portion of pillars of the first desorbent, the column into the upper portion 5 corn stover acid obtained in step b solution was discharged under Genzhu 1 ^ sugar solution, the sulfuric acid solution discharged brother 6 column, the desorbent flow rate of 3 billion • 5 m L / min, feed rate of 42_2mL / min, feed and desorption time wos after the completion of these three phases, a desorption stage and desorption stage feed inlet and outfeed sequentially moved backward to a column, and then repeated three stages each step, i.e., 8 8 steps to complete chromatography rotation i.e. two weeks post end of a cycle, then proceed to 下一个周期,方法与第一个周期相同,依次循环,直到分离过程达到稳态。分离得到的硫酸溶液浓度为230mg/mL、纯度为93.1%,收率为93 •5%,糖溶液浓度为24.8mg/mL、纯度95 • 2%,收率为94.2%; The next cycle, in the same manner as the first cycle, in cycles, until a separation process reached a steady state concentration of the sulfuric acid solution was separated 230mg / mL, purity 93.1%, yield of 93 • 5%, the concentration of sugar solution 24.8mg / mL, purity 95 • 2%, yield 94.2%;

[0030] d、硫酸溶液浓缩回收:将经c步骤得到的硫酸溶液进行旋转蒸发处理,温度55〇c, 得到浓缩液,再将其重复进行玉米秸秆酸解实验; [0030] d, and concentrated sulfuric acid solution recovered: a rotary evaporator will be treated with a sulfuric acid solution obtained in step c, 55〇c temperature, to obtain a concentrate, and then repeated the experiment for corn stover acid hydrolysis;

[0031] e、糖溶液过滤:将c步骤制得糖溶液用微米级滤器进行过滤,制得澄清的黄色液体; [0031] e, sugar solution filtered: The sugar solution prepared in step c was filtered through a micron filter, to obtain a clear yellow liquid;

[0032] f、糖溶液浓缩:将e步骤制得糖溶液进行旋转蒸发处理,温度为60〜65〇C,制得澄清的黄色液体; [0032] f, concentrated sugar solution: The sugar solution obtained in step e by rotary evaporation process, the temperature is 60~65〇C, prepared as a clear yellow liquid;

[0033] 实施例2: [0033] Example 2:

[0034]这种顺序式模拟移动床分离玉米猜杆酸解液中糖酸的方法如下: [0034] The method of acid hydrolysis of corn lever guess liquid sugar acids such sequential simulated moving bed separation as follows:

[0035] a、玉米秸秆酸解液的制备:将玉米秸秆烘干、粉碎,称取一定质量玉米秸杆,按照料液比1:5〇比例添加体积浓度3%的硫酸溶液,置于微波萃取仪中,调整微波功率700W,温度80°C,反应153min,得到玉米秸秆酸解液。 [0035] a, Preparation of corn stover hydrolyzate acid: corn stover drying, grinding, weighed certain quality corn stover, according to liquid ratio 1: 5〇 ratio of added concentration of 3 vol% sulfuric acid solution, placed in a microwave extraction apparatus, adjusting the microwave power 700W, a temperature of 80 ° C, the reaction 153min, corn stover to give the acid hydrolyzate.

[0036] b、用滤纸将a步骤制得的玉米秸杆酸解液过滤,得到澄清深棕色液体,并利用旋转蒸发仪将其浓缩至溶液中硫酸浓度562 • 3mg/mL、糖液浓度65.8mg/mL。 [0036] b, the step of using a filter paper made of corn stover acid solution was filtered to give a clear dark brown liquid, using a rotary evaporator and concentrated to a sulfuric acid concentration in the solution 562 • 3mg / mL, sugar concentration 65.8 mg / mL.

[0037] c、顺序式模拟移动床分离:处理后的玉米秸秆酸解液通过顺序式模拟移动床色谱^备进行分离,吸附剂为阳离子交换树脂IRl2〇H+;解吸剂为去离子水,分离温度为55。 [0037] c, sequential simulated moving bed separation: acid hydrolysis of corn stover was treated by sequential simulated moving bed chromatographic separation apparatus ^, the adsorbent is a cation exchange resin IRl2〇H +; desorbent deionized water, separated temperature was 55. (:,分离过程一个周期包括8步,每个步骤包括三个阶段,第一阶段为分离阶段,8根色谱柱串联连接,由安装在第3柱下的循环栗将柱中液体抽出注入第4根柱,第4根柱中液体注入第5根柱中,依次往复进行循环操作,循环量为435mL;第二阶段为解吸阶段,在第1根柱上部进入解吸剂,第6根柱下放出硫酸溶液,解吸剂流量为25 • lmL/min,解吸时间为123s;第三阶段为进料解吸阶段,在第1根柱上部进入解吸剂,第5根色谱柱上部进入b步骤所得玉米秸秆酸解液,第1根柱下放出糖溶液,第6根色谱柱下放出硫酸溶液,解吸剂流量为30. lmL/min,进料量为43_5mL/min,进料和解吸时间为179s。这三个阶段完成后,解吸阶段和进料解吸阶段的进料口和出料口都依次向后移动一个色谱柱,再重复进行每个步骤的三个阶段,8步完成即8根色谱柱轮换一周即一个周期结束,接下来进入 (:, The separation process comprises a cycle of eight steps, each step comprising three stages, the first stage is a separation stage, eight columns are connected in series, mounted in a loop of Li 3 post injection the column of liquid withdrawn four column, four column of the liquid injection 5 Genzhu sequentially reciprocated cycle of operation, the circulating volume of 435 mL; the second stage desorption stage, the upper portion of pillars into the first desorbent, the sixth Genzhu sulfuric acid solution discharged, the desorbent flow rate of 25 • lmL / min, desorption time is 123S; the third stage of the desorption stage feed, enter the upper portion of pillars of the first desorbent, the column into the upper portion 5 from step b corn stover acid hydrolysis solution, discharged under Genzhu first sugar solution, the sulfuric acid solution discharged under six columns, the desorbent flow rate of 30. lmL / min, feed rate of 43_5mL / min, feed and desorption time of 179s. this after three stages, desorption stage and desorption stage feed inlet and outfeed sequentially moved backward to a column, and then repeated three stages each step, i.e., the completion of step 8 8 column rotation That is the end of a period of one week, then enter 一个周期,方法与第一个周期相同,依次循环,直到分离过程达到稳态。分离得到的硫酸溶液浓度为241mg/mL、纯度为94%,收率为95.2%,糖溶液浓度为26.3mg/mL、纯度93.5%,收率为94.6%; A cycle, the first cycle in the same manner, in cycles, until a separation process reached a steady state concentration of the sulfuric acid solution was separated 241mg / mL, 94% purity, yield 95.2% sugar solution at a concentration of 26.3mg / mL, purity 93.5%, yield 94.6%;

[0038] d、硫酸溶液浓缩回收:将经c步骤得到的硫酸溶液进行旋转蒸发处理,温度55。 [0038] d, and concentrated sulfuric acid solution recovered: a rotary evaporator will be treated with a sulfuric acid solution obtained in step c, a temperature of 55. 〇, 得到浓缩液,再将其重复进行玉米秸杆酸解实验; Square, to obtain a concentrate, which is then acid hydrolysis of corn stover repeated experiments;

[0039] e、糖溶液过滤:将c步骤制得糖溶液用微米级滤器进行过滤,制得澄清的黄色液体; [0039] e, sugar solution filtered: The sugar solution prepared in step c was filtered through a micron filter, to obtain a clear yellow liquid;

[0040] f、糖溶液浓缩:将e步骤制得糖溶液进行旋转蒸发处理,温度为6〇〜65。 [0040] f, concentrated sugar solution: The sugar solution obtained in step e by rotary evaporation process, the temperature is 6〇~65. 〇,制得澄清的黄色液体; Square, prepared as a clear yellow liquid;

[0041] 实施例3: [0041] Example 3:

[0042]这种顺序式模拟移动床分离玉米猜杆酸解液中糖酸的方法如下: [0042] The method of acid hydrolysis of corn lever guess liquid sugar acids such sequential simulated moving bed separation as follows:

[0043] a、玉米秸秆酸解液的制备:将玉米秸杆烘干、粉碎,称取一定质量玉米秸杆,按照料液比1:50比例添加体积浓度3%的硫酸溶液,置于微波萃取仪中,调整微波功率700W,温度80°C,反应153min,得到玉米秸杆酸解液。 [0043] a, Preparation of Acid Hydrolyzate corn stover: The corn stover drying, grinding, weighed certain quality corn stover, adding a concentration of 3 vol% sulfuric acid solution according to ratio of solid to liquid ratio of 1:50, placed in a microwave extraction apparatus, adjusting the microwave power 700W, a temperature of 80 ° C, the reaction 153min, to give an acid hydrolyzate of corn stover.

[0044] b、用滤纸将a步骤制得的玉米秸秆酸解液过滤,得到澄清深棕色液体,并利用旋转蒸发仪将其浓缩至溶液中硫酸浓度616. lmg/mL、糖液浓度70.2mg/mL。 [0044] b, the step of using a filter paper made of corn stover acid solution was filtered to give a clear dark brown liquid, using a rotary evaporator and concentrated to mL, sugar concentration of sulfuric acid concentration in the solution 616. lmg / 70.2mg / mL.

[0045] ◦、顺序式模拟移动床分离:处理后的玉米秸杆酸解液通过顺序式模拟移动床色谱设备进行分离,吸附剂为阳离子交换树脂IR118H+;解吸剂为去离子水,分离温度为55。 [0045] ◦, sequential simulated moving bed separation: acid hydrolysis of corn stover was treated by sequential simulated moving bed chromatographic separation device, the adsorbent is a cation exchange resin IR118H +; desorbent is deionized water, for the separation temperature 55. (:,分离过程一个周期包括8步,每个步骤包括三个阶段,第一阶段为分离阶段,8根色谱柱串联连接,由安装在第3柱下的循环泵将柱中液体抽出注入第4根柱,第4根柱中液体注入第5根柱中,依次往复进行循环操作,循环量为428mL;第二阶段为解吸阶段,在第1根柱上部进入解吸剂,第6根柱下放出硫酸溶液,解吸剂流量为对• 5mL/min,解吸时间为112s;第三阶段为进料解吸阶段,在第1根柱上部进入解吸剂,第5根色谱柱上部进入b步骤所得玉米秸秆酸解液,第1根柱下放出糖溶液,第6根色谱柱下放出硫酸溶液,解吸剂流量为34.5mL/min,进料量为36_4mL/min,进料和解吸时间为12k。这三个阶段完成后,解吸阶段和进料解吸阶段的进料口和出料口都依次向后移动一个色谱柱,再重复进行每个步骤的三个阶段,8步完成即8根色谱柱轮换一周即一个周期结束,接下来进入下 (:, The separation process comprises a cycle of eight steps, each step comprising three stages, the first stage is a separation stage, eight columns are connected in series, a circulation pump is mounted in the third column of the column of liquid withdrawn injection four column, four column of the liquid injection 5 Genzhu sequentially reciprocated cycle of operation, the circulating volume of 428 mL; the second stage desorption stage, the upper portion of pillars into the first desorbent, the sixth Genzhu sulfuric acid solution discharged, the flow rate for the desorbent • 5mL / min, desorption time is 112S; the third stage of the desorption stage feed, enter the upper portion of pillars of the first desorbent, the column into the upper portion 5 from step b corn stover acid hydrolysis solution, discharged under Genzhu first sugar solution, the sulfuric acid solution discharged under six columns, the desorbent flow rate of 34.5mL / min, feed rate of 36_4mL / min, feed and desorption time 12k. three after the completion phase, the desorption phase and desorption phase of the feed inlet and outlet are sequentially moved backward to a column, and then repeated three stages each step, i.e., the completion of step 8 columns 8 rotate one week That is the end of a cycle, then go to the next 一个周期,方法与第一个周期相同,依次循环,直到分离过程达到稳态。分离得到的硫酸溶液浓度为318.6mg/mL、纯度为97.8%,收率为98%,糖溶液浓度为40 • 5mg/mL、纯度95%,收率为97%; A cycle, the first cycle in the same manner, in cycles, until a separation process reached a steady state concentration of sulfuric acid was separated from the solution obtained 318.6mg / mL, purity 97.8%, yield of 98% sugar solution at a concentration of 40 • 5mg / mL, 95% purity, 97% yield;

[0046] d、硫酸溶液浓缩回收:将经c步骤得到的硫酸溶液进行旋转蒸发处理,温度55, 得到浓缩液,再将其重复进行玉米秸杆酸解实验; [0046] d, and concentrated sulfuric acid solution recovered: a rotary evaporator will be treated with a sulfuric acid solution obtained in step c, a temperature of 55 to obtain a concentrate, and then repeated the experiment for corn stover acid hydrolysis;

[0047] e、糖溶液过滤:将c步骤制得糖溶液用微米级滤器进行过滤,制得澄清的黄色液体; [0047] e, sugar solution filtered: The sugar solution prepared in step c was filtered through a micron filter, to obtain a clear yellow liquid;

[0048] f、糖溶液浓缩:将e步骤制得糖溶液进行旋转蒸发处理,温度为60〜651,制得澄清的黄色液体; [0048] f, concentrated sugar solution: The sugar solution obtained in step e by rotary evaporation process, a temperature of 60~651, prepared as a clear yellow liquid;

[0049] 实施例4: [0049] Example 4:

[0050]这种顺序式模拟移动床分离玉米秸秆酸解液中糖酸的方法如下: [0050] The method of acid hydrolysis of corn stalk liquid sugar acids such sequential simulated moving bed separation as follows:

[0051 ] a、玉米秸杆酸解液的制备:将玉米秸秆烘干、粉碎,称取一定质量玉米秸杆,按照料液比1:50比例添加体积浓度3%的硫酸溶液,置于微波萃取仪中,调整微波功率700W,温度80°C,反应153min,得到玉米秸秆酸解液。 [0051] a, preparation of an acid hydrolyzate of corn stover: The corn stover drying, grinding, weighed certain quality corn stover, adding a concentration of 3 vol% sulfuric acid solution in accordance with the ratio of solid to liquid ratio of 1:50, placed in a microwave extraction apparatus, adjusting the microwave power 700W, a temperature of 80 ° C, the reaction 153min, corn stover to give the acid hydrolyzate.

[0052] b、用滤纸将a步骤制得的玉米秸杆酸解液过滤,得到澄清深棕色液体,并利用旋转蒸发仪将其浓缩至溶液中硫酸浓度546.8mg/mL、糖液浓度63.4mg/mL。 [0052] b, the step of using a filter paper made of corn stover acid solution was filtered to give a clear dark brown liquid, using a rotary evaporator and concentrated to a sulfuric acid concentration in the solution 546.8mg / mL, sugar concentration 63.4mg / mL.

[0053] c、顺序式模拟移动床分离:处理后的玉米秸秆酸解液通过顺序式模拟移动床色谱设,进行分离,吸附剂为阳离子交换树脂IR120Na+;解吸剂为去离子水,分离温度为52°C, 分离过程一个周期包括8步,每个步骤包括三个阶段,第一阶段为分离阶段,8根色谱柱串联连接,由安装在第3柱下的循环泵将柱中液体抽出注入第4根柱,第4根柱中液体注入第5根柱中,依次往复进行循环操作,循环量为430mL;第二阶段为解吸阶段,在第1根柱上部进入解吸剂,第6根柱下放出硫酸溶液,解吸剂流量为25 • 8mL/min,解吸时间为131 s;第三阶段为进料解吸阶段,在第1根柱上部进入解吸剂,第5根色谱柱上部进入b步骤所得玉米秸秆酸解液,第1根柱下放出糖溶液,第6根色谱柱下放出硫酸溶液,解吸剂流量为35.6mL/rain,进料量为40_5mL/min,进料和解吸时间为156s。 [0053] c, sequential simulated moving bed separation: corn stover acid hydrolyzate treated by sequential simulated moving bed chromatography provided for separation, the adsorbent is a cation exchange resin IR120Na +; desorbent deionized water, separation temperature is 52 ° C, the separation process comprises a cycle of eight steps, each step comprising three stages, the first stage is a separation stage, eight columns are connected in series, a circulation pump is mounted in the third column of the withdrawn liquid column injection the first four column, four column of the liquid injection 5 Genzhu sequentially reciprocated cycle of operation, the circulating volume of 430 mL; the second stage desorption stage, the upper portion of pillars into the first desorbent, 6 Genzhu releasing the sulfuric acid solution, the desorbent flow rate of 25 • 8mL / min, desorption time of 131 s; third stage is fed desorption phase, in the upper portion of pillars into the first desorbent, the column into the upper portion 5 obtained in step b corn stover acid hydrolyzate, Genzhu released under a first sugar solution, the sulfuric acid solution discharged under six columns, the desorbent flow rate of 35.6mL / rain, feeding amount 40_5mL / min, feed and desorption time of 156s. 这三个阶段完成后,解吸阶段和进料解吸阶段的进料口和出料口都依次向后移动一个色谱柱,再重复进行每个步骤的三个阶段,8步完成即8根色谱柱轮换二周即一个周期结束,接下来进入下一个周期,方法与第一个周期相同,依次循环,直到分离过程达到稳态。 After completion of the three stages, desorption stage and desorption stage feed inlet and outfeed sequentially moved backward to a column, and then repeated three stages each step, i.e., the completion of step 8 8 column i.e., two weeks rotation period is completed, then the next cycle, in the same manner as the first cycle, in cycles, until a separation process reached a steady state. 分离得到的硫酸溶液浓度为214mg/mL、纯度为95.2%,收率为% • 2%,糖溶液浓度为23 • 4mg/mL、纯度94 • 6%,收率为94.8%; A sulfuric acid concentration solution obtained was isolated 214mg / mL, purity 95.2%, yield% • 2%, concentration of the sugar solution is a 23 • 4mg / mL, purity 94 • 6%, a yield of 94.8%;

[0054] d、硫酸溶液浓缩回收:将经c步骤得到的硫酸溶液进行旋转蒸发处理,温度55。 [0054] d, and concentrated sulfuric acid solution recovered: a rotary evaporator will be treated with a sulfuric acid solution obtained in step c, a temperature of 55. (:, 得到浓缩液,再将其重复进行玉米秸秆酸解实验; (:, To obtain a concentrate, which is then acid hydrolysis of corn stover repeated experiments;

[0055] e、糖溶液过滤:将c步骤制得糖溶液用微米级滤器进行过滤,制得澄清的黄色液体; [0055] e, sugar solution filtered: The sugar solution prepared in step c was filtered through a micron filter, to obtain a clear yellow liquid;

[0056] f、糖溶液浓缩:将e步骤制得糖溶液进行旋转蒸发处理,温度为6〇〜65<>c,制得澄清的黄色液体; [0056] f, concentrated sugar solution: The sugar solution obtained in step e by rotary evaporation process, the temperature is 6〇~65 <> c, to obtain a clear yellow liquid;

[0057] 实施例5: [0057] Example 5:

[0058]这种顺序式模拟移动床分离玉米猜杆酸解液中糖酸的方法如下: [0058] The method of acid hydrolysis of corn lever guess liquid sugar acids such sequential simulated moving bed separation as follows:

[0059] a、玉米秸秆酸解液的制备:将玉米秸杆烘干、粉碎,称取一定质量玉米秸杆,按照料液比1:5〇比例添加体积浓度3%的硫酸溶液,置于微波萃取仪中,调整微波功率700¥,温度8〇°C,反应l53min,得到玉米稻秆酸解液。 [0059] a, Preparation of corn stover hydrolyzate acid: The corn stover drying, grinding, weighed certain quality corn stover, according to liquid ratio 1: 5〇 concentration of 3% by volume ratio of added sulfuric acid solution was placed microwave extraction instrument, ¥ 700 to adjust the microwave power, temperature 8〇 ° C, the reaction l53min, to give an acid hydrolyzate of corn rice straw.

[0060] b、用滤纸将a步骤制得的玉米秸杆酸解液过滤,得到澄清深棕色液体,并利用旋转蒸发仪将其浓缩至溶液中硫酸浓度635 • 4mg/mL、糖液浓度73.5mg/mL。 [0060] b, the step of using a filter paper made of corn stover acid solution was filtered to give a clear dark brown liquid, using a rotary evaporator and concentrated to a sulfuric acid concentration in the solution 635 • 4mg / mL, sugar concentration 73.5 mg / mL.

[0061] 序式模拟移动床分离:处理后的玉米秸秆酸解液通过顺序式模拟移动床色谱设备进行。 [0061] The frame sequential simulated moving bed separation: acid hydrolysis of corn stover was treated by sequential simulated moving bed chromatography apparatus. 分离,吸附剂为阳离子交换树脂AMBERjET C1H+;解吸剂为去离子水,分离温度为55°C,分离过程一个周期包括8步,每个步骤包括三个阶段,第一阶段为分离阶段,8根色谱柱串联连接,由女装在第3柱下的循环泵将柱中液体抽出注入第4根柱,第4根柱中液体注入第5根柱中,依次往复进行循环操作,循环量为550mL;第二阶段为解吸阶段,在第1根柱上部进入解吸剂,第6根柱下放出硫酸溶液,解吸剂流量为32.5mL/min,解吸时间为146s;第三阶段为进料解吸阶段,在第1根柱上部进入解吸剂,第5根色谱柱上部进入b步骤所得玉米秸秆酸解液,第1根柱下放出糖溶液,第6根色谱柱下放出硫酸溶液,解吸剂流量为32.5mL/min, 进料量为41.3mL/niin,进料和解吸时间为162s。 Separating the adsorbent is a cation exchange resin AMBERjET C1H +; desorbent deionized water, separating temperature of 55 ° C, the separation process comprises a cycle of eight steps, each step comprising three stages, the first stage is a separation stage, 8 column are connected in series, a circulation pump women in the third column of the column of liquid withdrawn four column injection, the liquid injection four column 5 Genzhu sequentially reciprocated cycle of operation, the circulating volume of 550mL; the second stage of the desorption stage, the first desorbent into the upper portion of pillars, the sulfuric acid solution discharged under 6 Genzhu, desorbent flow rate of 32.5mL / min, desorption time is 146s; third stage is fed desorption phase, Genzhu into the upper portion of the first desorbent, the column into the upper portion 5 obtained in step b corn stover acid hydrolyzate, sugar solution discharged under Genzhu first, the sulfuric acid solution discharged under six columns, the desorbent flow 32.5mL / min, feed rate of 41.3mL / niin, feed and desorption time of 162s. 这三个阶段完成后,解吸阶段和进料解吸阶段的进料口和出料口都依次向后移动一个色谱柱,再重复进行每个步骤的三个阶段,8步完成即8根色谱柱轮换一周即一个周期结束,接下来进入下一个周期,方法与第一个周期相同,依次循环,直到分离过程达到稳态。 After completion of the three stages, desorption stage and desorption stage feed inlet and outfeed sequentially moved backward to a column, and then repeated three stages each step, i.e., the completion of step 8 8 column i.e. the end of a one week period of rotation, then the next cycle, in the same manner as the first cycle, in cycles, until a separation process reached a steady state. 分离得到的硫酸溶液浓度为264mg/mL、纯度为93.4%,收率为94 • 3%,糖溶液浓度为32.4mg/mL、纯度94.9%,收率为96.2%; A sulfuric acid concentration solution obtained was isolated 264mg / mL, purity 93.4%, yield of 94 • 3%, sugar solution at a concentration of 32.4mg / mL, purity 94.9%, yield 96.2%;

[0062] d、硫酸溶液浓缩回收:将经c步骤得到的硫酸溶液进行旋转蒸发处理,温度55°C, 得到浓缩液,再将其重复进行玉米秸秆酸解实验; [0062] d, and concentrated sulfuric acid solution recovered: a rotary evaporator will be treated with a sulfuric acid solution obtained in step c, a temperature of 55 ° C, to obtain a concentrate, and then repeated the experiment for corn stover acid hydrolysis;

[0063] e、糖溶液过滤:将c步骤制得糖溶液用微米级滤器进行过滤,制得澄清的黄色液体; [0063] e, sugar solution filtered: The sugar solution prepared in step c was filtered through a micron filter, to obtain a clear yellow liquid;

[0064] f、糖溶液浓缩:将e步骤制得糖溶液进行旋转蒸发处理,温度为㈤〜65°C,制得澄清的黄色液体。 [0064] f, concentrated sugar solution: The sugar solution obtained in step e by rotary evaporation process, temperature ㈤~65 ° C, to obtain a clear yellow liquid.

[0065]本发明中料液比为质量体积比。 [0065] In the present invention, the mass ratio of solid to liquid volume ratio.

Claims (4)

  1. 1.一种)頓序式模拟移动床分离玉米秸秆酸解液中硫酸和糖液的方法,其特征在于:这种顺/宇式模拟移动床分离玉米秸秆酸解液中硫酸和糖液的方法,以玉米秸杆酸解液为原料•,采用顺序式模拟移动床分离设备分离硫酸和糖液,玉米秸秆酸解液中硫酸含量5〇〇mg/ ml〜700mg/ml、糖液含量6〇mg/mi〜80mg/mi;具体如下: _ 顺序式模拟移动床分离:将所述玉米秸秆酸解液通过顺序式模拟移动床色谱设备进行分离,分离过程一个周期包括8步,每个步骤包括三个阶段,第一阶段为分离阶段,8根色i普柱串联连接,由安装在第3柱下的循环泵将柱中液体抽出注入第4根柱,第4根柱中液体注入第5根柱中,依次往复进行循环操作;第二阶段为解吸阶段,在第丨根柱上部进入解吸剂, 第6根柱下放出硫酸溶液;第三阶段为进料解吸阶段,在第1根柱上部进入解吸剂,第5根色谱柱 Method corn stalk sulfuric acid solution and sugar mixture 1. A) Sequence of formula Dayton simulated moving bed separation, characterized in that: This cis / Yu formula simulated moving bed separation corn stalk acid solution and sulfuric acid solution of sugar A method for the acid hydrolyzate of corn stover feedstock •, using sequential simulated moving bed separation apparatus for separating sulfuric acid and sugar, corn stover hydrolyzate content of sulfuric acid 5〇〇mg / ml~700mg / ml, 6 sugar content 〇mg / mi~80mg / mi; follows: _ sequential simulated moving bed separation: the acid hydrolysis of corn stover was isolated by sequential chromatographic simulated moving bed apparatus, a separation cycle comprising 8 steps, each step comprises three phases, the first separation stage is, eight-color i P column are connected in series, a circulation pump is mounted in the third column of the column of liquid injection extracted four column, four column of the liquid injection section 5 Genzhu sequentially reciprocated cycle of operation; and a second stage desorption stage, the first desorbent into the upper portion of pillars Shu, the sulfuric acid solution discharged under 6 Genzhu; third stage is fed desorption phase, the first one desorbent column portion, the column 5 部进入所述玉米秸杆酸解液,第1根柱下放出糖溶液,第6根色谱柱下放出硫酸溶液; 这三个阶段完成后,解吸阶段和进料解吸阶段的进料口和出料口都依次向后移动一个色谱柱,再重复进行每个步骤的三个阶段,8步完成即8根色谱柱轮换一周即一个周期结束,接下来进入下一个周期,方法与第一个周期相同,依次循环,直到分离过程达到稳态;分离得到的硫酸溶液浓度为210mg/mL〜32〇mg/mL、纯度为93%〜98%,糖溶液浓度为20mg/mL〜41mg/ mL、纯度93% 〜96%; b、 硫酸溶液浓缩回收:将经a步骤得到的硫酸溶液进行旋转蒸发处理,温度50 °C〜65 C,得到浓缩液,浓缩液浓度为5〇〇mg/mL〜550mg/mL; c、 糖溶液过滤:将a步骤制得糖溶液用微米级滤器进行过滤,制得澄清的黄色液体; d、 糖溶液浓缩:将c步骤制得糖溶液进行旋转蒸发处理,温度为6〇〜65°C,制得澄清的黄色液 Portion into the corn stover acid hydrolyzate, sugar solution discharged under Genzhu first, the sulfuric acid solution discharged under six columns; After these three stages, the desorption desorption stage and a feed stage and the feed inlet feed ports are successively moved backward to a column, and then repeated three stages each step, i.e., the completion of step 8 8 columns i.e. a rotation of one week period ends, then proceed to the next cycle, the first cycle method the same, in cycles, until a separation process reached a steady state; the concentration of sulfuric acid was separated from the solution obtained 210mg / mL~32〇mg / mL, purity of 93% ~98% sugar solution of a concentration of 20mg / mL~41mg / mL, purity 93% ~96%; b, and concentrated sulfuric acid solution recovered: a rotary evaporator will be treated with a sulfuric acid solution obtained in step, a temperature of 50 ° C~65 C, to obtain a concentrate, the concentrate concentration 5〇〇mg / mL~550mg / mL; c, sugar solution filtered: the a step to prepare a sugar solution was filtered using a micron filter to obtain a clear yellow liquid; D, a sugar solution was concentrated: the step c obtained saccharide solution was rotary evaporation process, the temperature is 6〇~65 ° C, to obtain a clear yellow solution .
  2. 2.根据权利要求1所述的顺序式模拟移动床分离玉米秸秆酸解液中硫酸和糖液的方法,其特征在于:所述的玉米秸秆酸解液的制备方法: 第一步、玉米秸杆酸解液的制备:将玉米秸杆烘干、粉碎过40目筛,称取2g玉米秸秆粉, 加入体积浓度3%的硫酸溶液100mL,置于微波萃取仪中,调整微波功率7〇〇w,温度8(TC,反应153min,得到玉米秸杆酸解液; 第二步、用滤纸将第一步制得的玉米秸秆酸解液过滤,得到澄清深棕色液体,并利用旋转蒸发仪将其浓缩至溶液中硫酸含量500mg/ml〜7〇〇mg/ml、糖液含量6〇mg/ml〜80mg/ml。 The sequential simulated moving bed method of claim 1 and a sulfuric acid solution of sugar corn stover was isolated as claimed in claim, characterized in that: the method of preparing the hydrolyzate of corn straw acid: The first step, corn stalks preparation of the acid hydrolyzate of the rod: the corn stover dried, sifted through a 40 mesh screen, weighed 2g corn stalk powder, was added sulfuric acid concentration of 3% by volume solution 100mL, placed in a microwave extraction device, adjusting the microwave power 7〇〇 w, temperature 8 (TC, the reaction 153min, to give an acid hydrolyzate of corn stover; a second step, with the filter paper was first step in acid hydrolysis of corn stover obtained was filtered to give a clear dark brown liquid, using a rotary evaporator concentrated sulfuric acid to the solution content of 500mg / ml~7〇〇mg / ml, sugar content 6〇mg / ml~80mg / ml.
  3. 3.根据权利要求2所述的顺序式模拟移动床分离玉米秸秆酸解液中硫酸和糖液的方法,其特征在于:所述的顺序式模拟移动床的分离中,吸附剂为阳离子交换树脂UBK08、 IR120H+、IR118 H+、IR120Na+或AMBERJET C1H+中的任何一种;解吸剂为去离子水,分离温度为5〇°C〜55°C,第一阶段循环量为410〜55〇mL;第二阶段,解吸剂流量为23〜45mL/min,解吸时间为110〜160s;第二阶段,解吸剂流量为30〜45mL/min,进料量为35〜50mL/min,进料和解吸时间为120〜180s。 The sequential simulated moving bed method of claim 2 and a sugar liquid sulfuric acid solution was separated corn stover claim, wherein: said separate sequential simulated moving bed, the adsorbent is a cation exchange resin UBK08, IR120H +, IR118 H +, or any IR120Na + in AMBERJET C1H +; desorbent deionized water, separation temperature of 5〇 ° C~55 ° C, the first phase of the cycle in an amount of 410~55〇mL; second phase, the desorbent flow 23~45mL / min, desorption time 110~160s; a second phase, the desorbent flow 30~45mL / min, feed rate of 35~50mL / min, feed and desorption time 120 ~180s.
  4. 4.根据权利要求3所述的顺序式模拟移动床分离玉米稻秆酸解液中硫酸和糖液的方法,其特征在于:所述的步骤b得到的硫酸浓缩液稀释得到体积浓度3%的硫酸溶液,重复用于玉米秸杆酸解液制备的第一步中。 The sequential simulated moving bed separation corn rice straw of claim 3 in an acid solution of sulfuric acid and sugar solutions Method as claimed in claim, wherein: the dilution of the concentrated sulfuric acid solution obtained in step b to give a concentration of 3% by volume sulfuric acid solution prepared in the first step is repeated for the acid hydrolyzate of corn stover.
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CN101029060A (en) * 2007-04-04 2007-09-05 牛继星 Hydrolysis for producing high-purity crystallized xylose from corn skin
CN101792822A (en) * 2010-03-30 2010-08-04 天津科技大学 Method for separating and purifying xylose and arabinose from hemicellulose acid hydrolysis liquid
CN102102116A (en) * 2010-12-21 2011-06-22 山东省鲁洲食品集团有限公司 Method for preparing high-purity crystalline dextrose from maize peel acid hydrolysis residues
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