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CN109970587A - A kind of L-aspartic acid separation and purification device and method for separation and purification of L-aspartic acid - Google Patents

A kind of L-aspartic acid separation and purification device and method for separation and purification of L-aspartic acid Download PDF

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CN109970587A
CN109970587A CN201910369761.7A CN201910369761A CN109970587A CN 109970587 A CN109970587 A CN 109970587A CN 201910369761 A CN201910369761 A CN 201910369761A CN 109970587 A CN109970587 A CN 109970587A
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aspartic acid
pipeline
separation
membrane filtration
liquid
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CN109970587B (en
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徐礼生
张兴桃
高贵珍
赵亮
曹稳根
段腾飞
夏秋霞
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Suzhou University
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    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C227/00Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
    • C07C227/38Separation; Purification; Stabilisation; Use of additives
    • C07C227/40Separation; Purification
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07BGENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
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Abstract

本发明公开一种L‑天冬氨酸分离提纯装置,包括酶液储罐,酶液储罐连通有柱层析分离装置,柱层析分离装置连通有滤膜过滤装置,滤膜过滤装置连通有浓缩结晶装置;柱层析分离装置包括液盘,液盘的顶部连通有若干个层析柱。本发明公开的上述装置解决了现有技术中采用萃取装置分离提纯L‑天冬氨酸具有收率底、成本高,污染大的技术问题。同时,本发明提供了一种分离提纯L‑天冬氨酸的方法,具体包括柱层析吸附、洗脱、微滤膜和纳滤膜过滤以及浓缩结晶四大步骤。本发明公开的技术方案不仅分离效率高,收率高,分离所得L‑天冬氨酸的纯度较大,同时,采用柱层析分离方式分离,污水、废气量少,减少了工业化生产污染,降低了环保处理成本。

The invention discloses an L-aspartic acid separation and purification device, comprising an enzyme liquid storage tank, the enzyme liquid storage tank is connected with a column chromatography separation device, the column chromatography separation device is connected with a membrane filter device, and the filter membrane filter device is connected with There is a concentration and crystallization device; the column chromatography separation device includes a liquid tray, and the top of the liquid tray is connected with several chromatography columns. The above-mentioned device disclosed in the present invention solves the technical problems of low yield, high cost and large pollution of using an extraction device to separate and purify L-aspartic acid in the prior art. At the same time, the present invention provides a method for separating and purifying L-aspartic acid, which specifically includes four steps of column chromatography adsorption, elution, microfiltration membrane and nanofiltration membrane filtration, and concentration and crystallization. The technical solution disclosed by the invention not only has high separation efficiency and high yield, but also has a relatively high purity of L-aspartic acid obtained by separation, and at the same time, adopts a column chromatography separation method to separate the amount of sewage and waste gas, and reduces industrial production pollution. Reduced environmental disposal costs.

Description

一种L-天冬氨酸分离提纯装置及其分离提纯L-天冬氨酸的 方法A kind of L-aspartic acid separation and purification device and its separation and purification of L-aspartic acid method

技术领域technical field

本发明涉及氨基酸提取柱层析分离装置,尤其涉及的是一种L-天冬氨酸分离提纯装置及其分离提纯L-天冬氨酸的方法。The invention relates to an amino acid extraction column chromatography separation device, in particular to an L-aspartic acid separation and purification device and a method for separating and purifying L-aspartic acid.

背景技术Background technique

L-天冬氨酸,其结构如下所示:L-Aspartic acid, whose structure is shown below:

L-天冬氨酸不仅可以为人体提供氨基酸源,且能够作为药用如氨解毒剂。关于L-天冬氨酸的工业化制备方法,现有技术大都采用化学合成的手段制备得到,但是化学合成的缺陷在于污染大。L-aspartic acid can not only provide amino acid source for the human body, but also can be used as an antidote for medicinal purposes such as ammonia. Regarding the industrialized preparation method of L-aspartic acid, the prior art is mostly prepared by means of chemical synthesis, but the defect of chemical synthesis is that the pollution is large.

为了克服化学合成L-天冬氨酸的技术缺陷,科研人员采用生物发酵的方法制备得到L-天冬氨酸前体的发酵液,再对发酵液酶解,得到富含L-天冬氨酸的控制酶转化液。然而,在生物发酵获得L-天冬氨酸的过程中,分离控制酶转化液中的L-天冬氨酸一直是难以解决的技术问题。In order to overcome the technical defects of chemical synthesis of L-aspartic acid, the researchers used the method of biological fermentation to prepare the fermentation liquid of L-aspartic acid precursor, and then enzymatically hydrolyzed the fermentation liquid to obtain L-aspartic acid rich in fermentation liquid. Acid-controlled enzymatic conversion solution. However, in the process of obtaining L-aspartic acid by biological fermentation, it has always been a difficult technical problem to separate and control the L-aspartic acid in the enzymatic transformation liquid.

现有技术中为了从控制酶转化液分离L-天冬氨酸,大都采用萃取手段,通过萃取的方式获取L-天冬氨酸。In the prior art, in order to separate L-aspartic acid from the control enzyme conversion liquid, extraction means are mostly used to obtain L-aspartic acid through extraction.

然而,对于上述萃取手段,由于控制酶转化液中除L-天冬氨酸外,还含有其他多种杂质,通过反复萃取,反复结晶的方式才能够获取L-天冬氨酸,通过上述反复萃取、结晶后得到的L-天冬氨酸收率异常低下。However, for the above-mentioned extraction method, since the control enzyme conversion solution contains various other impurities besides L-aspartic acid, L-aspartic acid can be obtained by repeated extraction and repeated crystallization. The yield of L-aspartic acid obtained after extraction and crystallization is abnormally low.

对于难以通过萃取手段分离提纯或者萃取手段分离收率低下,目前采用的是柱层析分离方式解决。For the difficulty of separation and purification by extraction means or the low separation yield of extraction means, column chromatography is currently used to solve the problem.

柱层析分离技术,即通过层析柱进行色谱分离,已经从实验室使用的小型层析柱应用到工业化分离生产的大型层析柱。分离液加入到大型层析柱内,层析柱内的吸附剂如硅胶等,将分离液中的物质进行层析分离。由于,工业化生产的大型层析柱具有一定的高度和宽度,其理论塔板数较大,分离效率高,同时,一次性分离所得量也较大。Column chromatographic separation technology, that is, chromatographic separation through chromatographic columns, has been applied from small chromatographic columns used in laboratories to large chromatographic columns produced by industrial separation. The separation liquid is added to a large-scale chromatography column, and the adsorbent in the chromatography column, such as silica gel, etc., separates the substances in the separation liquid by chromatography. Because the industrially produced large-scale chromatography column has a certain height and width, the number of theoretical plates is large, the separation efficiency is high, and at the same time, the amount of one-time separation is also large.

但是,至今未有一种能够适用于L-天冬氨酸的柱层析设备及适用的层析方法。现有技术中仍旧采用传统的多次萃取-结晶的技术进行分离,萃取方式产生的废液量较大,造成工业化污水处理成本较高,同时,萃取成本较大。However, up to now there is no column chromatography equipment and applicable chromatography method that can be applied to L-aspartic acid. In the prior art, the traditional multiple extraction-crystallization technology is still used for separation, and the amount of waste liquid produced by the extraction method is relatively large, resulting in high industrialized sewage treatment cost and high extraction cost.

发明内容SUMMARY OF THE INVENTION

本发明所要解决的技术问题在于提供了一种L-天冬氨酸分离提纯装置及其分离提纯L-天冬氨酸的方法。The technical problem to be solved by the present invention is to provide a L-aspartic acid separation and purification device and a method for separation and purification of L-aspartic acid.

本发明是通过以下技术方案解决上述技术问题的:The present invention solves the above-mentioned technical problems through the following technical solutions:

一种L-天冬氨酸分离提纯装置,包括酶液储罐,所述酶液储罐连通有柱层析分离装置,所述柱层析分离装置连通有滤膜过滤装置,所述滤膜过滤装置连通有浓缩结晶装置;An L-aspartic acid separation and purification device, comprising an enzyme liquid storage tank, the enzyme liquid storage tank is connected with a column chromatography separation device, and the column chromatography separation device is connected with a filter membrane filtration device, the filter membrane The filtering device is communicated with a concentration and crystallization device;

所述柱层析分离装置包括液盘,所述液盘的顶部连通有若干个层析柱,所述层析柱之间连通有第一管道,所述第一管道连通有第二管道,所述第二管道连通酶液储罐;The column chromatography separation device includes a liquid pan, the top of the liquid pan is connected with a plurality of chromatography columns, a first pipeline is connected between the chromatography columns, and the first pipeline is connected with a second pipeline, so the The second pipeline is communicated with the enzyme liquid storage tank;

所述液盘的底部连通有第三管道,所述第三管道连通滤膜过滤装置,所述滤膜过滤装置连通浓缩结晶装置;The bottom of the liquid pan is connected with a third pipeline, the third pipeline is connected with a membrane filtration device, and the membrane filtration device is connected with a concentration and crystallization device;

所述滤膜过滤装置包括微滤膜过滤装置和纳滤膜过滤装置,所述纳滤膜过滤装置的顶部和微滤膜过滤装置的顶部通过第五管道连通;The membrane filtration device includes a microfiltration membrane filtration device and a nanofiltration membrane filtration device, and the top of the nanofiltration membrane filtration device and the top of the microfiltration membrane filtration device are communicated through a fifth pipeline;

所述微滤膜过滤装置的底部连通第三管道,所述纳滤膜过滤装置的底部通过第四管道连通浓缩结晶装置;The bottom of the microfiltration membrane filtration device is communicated with the third pipeline, and the bottom of the nanofiltration membrane filtration device is communicated with the concentration and crystallization device through the fourth pipeline;

所述第一管道、第二管道、第三管道、第四管道,以及第五管道均设置有阀门。The first pipeline, the second pipeline, the third pipeline, the fourth pipeline, and the fifth pipeline are all provided with valves.

优选地,所述液盘的顶部对称分布有6个层析柱,所述层析柱以液盘的盘心为对称中心,对称分布在液盘底部的侧边位置;Preferably, six chromatography columns are symmetrically distributed on the top of the liquid pan, and the chromatography columns are symmetrically distributed on the side of the bottom of the liquid pan with the center of the liquid pan as the center of symmetry;

位于对角位置处的所述层析柱之间通过第一管道连通,所述第一管道之间相互贯穿连通,所述第一管道的贯穿处向上垂直连通第二管道。The chromatographic columns located at the diagonal positions are communicated with each other through first pipes, the first pipes are in penetrating communication with each other, and the penetrating parts of the first pipes are vertically connected to the second pipes upward.

优选地,所述第一管道两端的端部分别贯穿对应层析柱的顶部,所述第一管道的端部两端的端部分别连通有金属过滤球。Preferably, the ends of the two ends of the first pipe respectively penetrate through the top of the corresponding chromatography column, and the ends of the two ends of the first pipe are respectively connected with metal filter balls.

优选地,所述层析柱包括顶盖、底盖以及柱体,所述顶盖连接柱体的顶部,底盖连接柱体的底部,所述顶盖内设置有内腔,所述金属过滤球位于顶盖的内腔中,所述柱体内设置有层析空腔,所述层析空腔连通顶盖的内腔,所述层析空腔的腔顶位置连接有防冲击盘;Preferably, the chromatography column comprises a top cover, a bottom cover and a column body, the top cover is connected to the top of the column body, the bottom cover is connected to the bottom of the column body, the top cover is provided with an inner cavity, and the metal filter The ball is located in the inner cavity of the top cover, the column is provided with a chromatography cavity, the chromatography cavity is communicated with the inner cavity of the top cover, and an anti-impact disk is connected to the top of the chromatography cavity;

所述防冲击盘上开设有若干个通孔,所述通孔连通层析空腔,所述通孔上固定连接有滤网;A plurality of through holes are opened on the anti-shock disk, the through holes are connected to the chromatography cavity, and a filter screen is fixedly connected to the through holes;

所述底盖内设置有内腔,所述底盖的内腔连通层析空腔,所述底盖通过排液管连通在液盘的顶部,所述排液管设置有阀门。The bottom cover is provided with an inner cavity, the inner cavity of the bottom cover communicates with the chromatography cavity, and the bottom cover is communicated with the top of the liquid pan through a liquid drain pipe, and the liquid drain pipe is provided with a valve.

优选地,所述层析空腔填充有离子交换树脂。Preferably, the chromatography cavity is filled with ion exchange resin.

优选地,所述浓缩结晶装置包括浓缩结晶釜,所述浓缩结晶釜内设置有搅拌装置,所述浓缩结晶釜连通有真空装置。Preferably, the concentrated crystallization device comprises a concentrated crystallization kettle, a stirring device is arranged in the concentrated crystallization kettle, and a vacuum device is communicated with the concentrated crystallization kettle.

优选地,所述液盘内部中空,所述液盘的侧壁上设置有玻璃观察区。Preferably, the inside of the liquid pan is hollow, and a glass observation area is provided on the side wall of the liquid pan.

优选地,所述玻璃观察区上设有刻度标线。Preferably, scale markings are provided on the glass observation area.

优选地,所述液盘内的底部固定连接有一层圆形滤网,所述圆形滤网覆盖液盘内的底面。Preferably, a layer of circular filter screen is fixedly connected to the bottom of the liquid pan, and the circular filter screen covers the bottom surface of the liquid pan.

本发明同时公开采用上述L-天冬氨酸分离提纯装置分离提纯L-天冬氨酸的方法,包括以下步骤:The present invention also discloses a method for separating and purifying L-aspartic acid by adopting the above-mentioned L-aspartic acid separation and purification device, comprising the following steps:

S1、将50L,L-天冬氨酸浓度含量为160-210g/L的调节酶转化液泵入到酶液储罐中,调节调节酶转化液的pH至4-8后,打开阀门,将调节酶转化液加入至柱层析分离装置中吸附,L-天冬氨酸吸附在柱层析分离装置中,控制调节酶转化液流入柱层析分离装置中的流速为100-2000mL/min;S1, pump 50L, L-aspartic acid concentration content of 160-210g/L regulating enzyme transformation liquid into the enzyme liquid storage tank, after adjusting the pH of regulating enzyme transformation liquid to 4-8, open the valve, The regulating enzyme conversion solution is added to the column chromatography separation device for adsorption, and L-aspartic acid is adsorbed in the column chromatography separation device, and the flow rate of the regulating enzyme conversion solution flowing into the column chromatography separation device is controlled to be 100-2000 mL/min;

S2、吸附完毕,将氢氧化钠溶液泵入至酶液储罐中,作为洗脱液,打开阀门,利用氢氧化钠洗脱柱层析分离装置中吸附的L-天冬氨酸,控制氢氧化钠的洗脱流速为100-2000mL/min;S2. After the adsorption, the sodium hydroxide solution is pumped into the enzyme liquid storage tank, as the eluent, the valve is opened, and the L-aspartic acid adsorbed in the column chromatography separation device is eluted with sodium hydroxide to control the hydrogen The elution flow rate of sodium oxide is 100-2000mL/min;

S3、洗脱过程中,打开阀门,洗脱液依次进入微滤膜过滤装置和纳滤膜过滤装置过滤后,进入浓缩结晶装置内;S3. During the elution process, open the valve, and the eluent enters the microfiltration membrane filtration device and the nanofiltration membrane filtration device in turn, and then enters the concentrated crystallization device;

S4、减压浓缩洗脱液后,加硫酸调浓缩液的pH值为1.5-3.0后,加入L-天冬氨酸晶种,进行结晶,经过滤、烘干后,得到L-天冬氨酸纯品。S4, after concentrating the eluent under reduced pressure, adding sulfuric acid to adjust the pH value of the concentrated solution to 1.5-3.0, adding L-aspartic acid seed crystals to crystallize, and after filtering and drying to obtain L-aspartic acid Pure acid.

本发明相比现有技术具有以下优点:Compared with the prior art, the present invention has the following advantages:

本发明公开的装置解决了现有技术中以萃取手段分离提纯L-天冬氨酸具有收率底、成本高,污染大的技术问题。本发明公开的装置提供一种适用于工业化柱层析分离L-天冬氨酸装置,采用上述装置进行柱层析分离L-天冬氨酸,不仅分离效率高,收率高,分离所得L-天冬氨酸的纯度也较大,同时,采用柱层析分离方式分离,污水、废气量少,减少了工业化污染,降低了环保处理成本。The device disclosed by the invention solves the technical problems of low yield, high cost and large pollution in the prior art by extracting and purifying L-aspartic acid. The device disclosed in the present invention provides a device suitable for industrial column chromatography separation of L-aspartic acid. Using the above device to separate L-aspartic acid by column chromatography not only has high separation efficiency and high yield, but also obtains L-aspartic acid. -The purity of aspartic acid is also relatively high. At the same time, the separation method is adopted by column chromatography, and the amount of sewage and waste gas is small, which reduces industrial pollution and reduces the cost of environmental protection treatment.

本发明公开的分离提纯方法,替代传统工业化使用的萃取方法,具有收率高、纯度达到99.9%,且方法简单的优点。The separation and purification method disclosed by the invention replaces the extraction method used in traditional industrialization, and has the advantages of high yield, 99.9% purity and simple method.

附图说明Description of drawings

图1是本发明实施例的整体结构示意图;Fig. 1 is the overall structure schematic diagram of the embodiment of the present invention;

图2是本发明实施例中浓缩结晶装置与滤膜过滤装置的结构示意图;Fig. 2 is the structural representation of the concentrated crystallization device and the membrane filtration device in the embodiment of the present invention;

图3是本发明实施例中柱层析分离装置的结构示意图;Fig. 3 is the structural representation of the column chromatography separation device in the embodiment of the present invention;

图4是本发明实施例中层析柱的截面图;4 is a cross-sectional view of a chromatography column in an embodiment of the present invention;

图5是本发明实施例中图4中A部位的局部放大结构示意图;Fig. 5 is the partial enlarged structural schematic diagram of the part A in Fig. 4 in the embodiment of the present invention;

图6是本发明实施例中防冲击盘的结构示意图;6 is a schematic structural diagram of an anti-shock disc in an embodiment of the present invention;

图7是本发明实施例中第一管道和第二管道的连接关系图;Fig. 7 is the connection relation diagram of the first pipeline and the second pipeline in the embodiment of the present invention;

图8是本发明实施例2中结晶得到L-天冬氨酸纯品的红外检测谱图。Fig. 8 is the infrared detection spectrum of pure L-aspartic acid obtained by crystallization in Example 2 of the present invention.

具体实施方式Detailed ways

下面对本发明的实施例作详细说明,本实施例在以本发明技术方案为前提下进行实施,给出了详细的实施方式和具体的操作过程,但本发明的保护范围不限于下述的实施例。The embodiments of the present invention are described in detail below. This embodiment is implemented on the premise of the technical solution of the present invention, and provides a detailed implementation manner and a specific operation process, but the protection scope of the present invention is not limited to the following implementation. example.

实施例1L-天冬氨酸分离提纯装置Example 1L-Aspartic acid separation and purification device

如图1--7所示,一种L-天冬氨酸分离提纯装置,包括酶液储罐1,酶液储罐1连通有柱层析分离装置2(柱层析分离装置2位于酶液储罐1的下方),柱层析分离装置2连通有滤膜过滤装置3(滤膜过滤装置3位于柱层析分离装置2的下方),滤膜过滤装置3连通有浓缩结晶装置4(浓缩结晶装置4位于滤膜过滤装置3的下方)。As shown in Figure 1--7, a kind of L-aspartic acid separation and purification device, comprises enzyme liquid storage tank 1, and enzyme liquid storage tank 1 is communicated with column chromatography separation device 2 (column chromatography separation device 2 is located in the enzyme liquid storage tank 1). The bottom of the liquid storage tank 1), the column chromatography separation device 2 is communicated with a membrane filter device 3 (the membrane filter device 3 is located below the column chromatography separation device 2), and the membrane filter device 3 is communicated with a concentrated crystallization device 4 ( The concentration crystallization device 4 is located below the membrane filtration device 3).

上述装置中:滤膜过滤装置3包括微滤膜过滤装置31和纳滤膜过滤装置32(微滤膜过滤装置31和纳滤膜过滤装置32相互连通),其中,微滤膜过滤装置31和纳滤膜过滤装置32为现有技术公开的常规微滤膜过滤设备和纳滤膜过滤设备,其主体结构包括对应的微滤膜以及纳滤膜,本领域技术人员通过查阅技术手册或者技术词典即可获知本发明公开的微滤膜过滤装置31和纳滤膜过滤装置32的具体结构和工作原理。In the above-mentioned device: the membrane filtration device 3 includes a microfiltration membrane filtration device 31 and a nanofiltration membrane filtration device 32 (the microfiltration membrane filtration device 31 and the nanofiltration membrane filtration device 32 communicate with each other), wherein, the microfiltration membrane filtration device 31 and The nanofiltration membrane filtration device 32 is the conventional microfiltration membrane filtration equipment and nanofiltration membrane filtration equipment disclosed in the prior art, and its main structure includes the corresponding microfiltration membrane and nanofiltration membrane. The specific structure and working principle of the microfiltration membrane filtration device 31 and the nanofiltration membrane filtration device 32 disclosed in the present invention can be known.

同时,浓缩结晶装置4为现有技术公开的常规浓缩结晶釜,其主体结构包括釜体,设置在釜体上的搅拌装置,以及连通在釜体顶部的真空装置,如真空泵,利用真空装置将釜体内的洗脱液进行浓缩。Meanwhile, the concentrated crystallization device 4 is a conventional concentrated crystallization kettle disclosed in the prior art, and its main structure includes a kettle body, a stirring device arranged on the kettle body, and a vacuum device connected to the top of the kettle body, such as a vacuum pump, which utilizes the vacuum device to The eluate in the kettle is concentrated.

本发明的改进点在于:The improvement point of the present invention is:

设置柱层析分离装置2,具体而言,柱层析分离装置2包括液盘22(液盘22内部中空,液盘22的侧壁上设置有玻璃观察区,玻璃观察区采用钢化玻璃设置,玻璃观察区上设有刻度标线221,利用刻度标线221标记液盘22内的液位),液盘22的顶部对称分布有6个层析柱21(每个层析柱21的长度为6.5m,半径为1m),层析柱21以液盘22的盘心为对称中心,对称分布在液盘22顶部的侧边位置。层析柱21的底部连通液盘22(层析柱21的底部连通一根排液管,排液管连通液盘22)。A column chromatography separation device 2 is provided, specifically, the column chromatography separation device 2 includes a liquid pan 22 (the interior of the liquid pan 22 is hollow, and a glass observation area is provided on the side wall of the liquid pan 22, and the glass observation area is set with tempered glass, The glass observation area is provided with a scale mark 221, and the scale mark 221 is used to mark the liquid level in the liquid pan 22), and the top of the liquid pan 22 is symmetrically distributed with 6 chromatography columns 21 (the length of each chromatography column 21 is 6.5m, the radius is 1m), the chromatography column 21 takes the center of the liquid pan 22 as the center of symmetry, and is symmetrically distributed on the side of the top of the liquid pan 22 . The bottom of the chromatography column 21 is connected to the liquid pan 22 (the bottom of the chromatography column 21 is connected to a drain pipe, and the drain pipe is connected to the liquid pan 22).

位于对角位置处的两个层析柱21(两个层析柱21分别位于一条直径线的两端)之间通过第一管道211连通(层析柱21的顶盖之间通过第一管道211连通),第一管道211之间交叉连通,第一管道211的交叉处向上垂直连通第二管道212。(同时,每个第一管道211均设置2个阀门,阀门分别位于第一管道211两端靠近层析柱21上顶盖201所在位置)。The two chromatographic columns 21 located at the diagonal positions (the two chromatographic columns 21 are located at two ends of a diameter line respectively) are communicated through the first pipeline 211 (the tops of the chromatographic columns 21 are connected through the first pipeline 211 connection), the first pipes 211 are cross-connected, and the intersection of the first pipes 211 is vertically connected to the second pipe 212 upward. (At the same time, each first pipe 211 is provided with two valves, and the valves are respectively located at both ends of the first pipe 211 near the position where the top cover 201 of the chromatography column 21 is located).

层析柱21的结构具体为:The structure of the chromatography column 21 is specifically:

层析柱21包括顶盖201、底盖202以及柱体,顶盖201连接柱体的顶部,底盖202连接柱体的底部,顶盖201内设置有内腔,第一管道211的两端的端部贯穿伸入到顶盖201的内腔中,并且端部连通一个金属过滤球2111(金属过滤球2111采用金属滤网编制而成,第一管道211的端部伸入到金属过滤球2111内,金属过滤球2111的目的是防止不溶物进入到层析空腔内,影响层析效果)。The chromatography column 21 includes a top cover 201, a bottom cover 202, and a column. The top cover 201 is connected to the top of the column, the bottom cover 202 is connected to the bottom of the column, and the top cover 201 is provided with an inner cavity. The end penetrates into the inner cavity of the top cover 201, and the end is connected to a metal filter ball 2111 (the metal filter ball 2111 is woven from a metal filter screen, and the end of the first pipe 211 extends into the metal filter ball 2111). , The purpose of the metal filter ball 2111 is to prevent insoluble matter from entering the chromatographic cavity and affect the chromatographic effect).

柱体内设置有层析空腔(层析空腔填充有离子交换树脂,离子交换树脂为732型阳离子交换树脂),层析空腔连通顶盖201的内腔,层析空腔的腔顶位置连接有防冲击盘213(防冲击盘213上开设有多个通孔2131,通孔2131连通层析空腔,通孔2131上固定连接有滤网,采用防冲击盘213设计的目的在于:防止洗脱液在加入到层析空腔一瞬间将填充的离子交换树脂粉末冲击变形)。先将离子交换树脂填充在层析空腔内,再将防冲击盘213螺接在层析空腔的腔口位置(防冲击盘213的侧壁上开设外螺纹部2132,对应的层析空腔的腔口内壁开设对应的内螺纹)。按照现有方式,将顶盖201与柱体设计成可拆卸方式连接,如将顶盖201螺接到柱体的顶部。The column is provided with a chromatography cavity (the chromatography cavity is filled with ion exchange resin, and the ion exchange resin is 732 type cation exchange resin), the chromatography cavity is connected to the inner cavity of the top cover 201, and the top position of the chromatography cavity The anti-shock plate 213 is connected (a plurality of through holes 2131 are opened on the anti-shock plate 213, the through holes 2131 are connected to the chromatography cavity, and the filter screen is fixedly connected to the through holes 2131. The purpose of using the anti-shock plate 213 is to prevent the Immediately after the eluent is added to the chromatographic cavity, the packed ion exchange resin powder is impacted and deformed). First fill the ion exchange resin in the chromatography cavity, and then screw the anti-shock disk 213 to the position of the cavity mouth of the chromatography cavity (an external thread portion 2132 is provided on the side wall of the anti-shock disk 213, and the corresponding chromatographic cavity The inner wall of the cavity of the cavity is provided with corresponding internal threads). According to the existing method, the top cover 201 and the cylinder are designed to be connected in a detachable manner, for example, the top cover 201 is screwed to the top of the cylinder.

同理,底盖202内设置有内腔,底盖202的内腔连通层析空腔,底盖202通过排液管连通在液盘22的顶部,排液管设置有阀门。Similarly, the bottom cover 202 is provided with an inner cavity, the inner cavity of the bottom cover 202 is connected to the chromatography cavity, the bottom cover 202 is connected to the top of the liquid pan 22 through a drain pipe, and the drain pipe is provided with a valve.

由于,位于对角位置处的两个层析柱21之间通过第一管道211连通,因此,6个层析柱21具有3个第一管道211,3个第一管道211位于同一水平面上,3个第一管道211之间具有交叉,交叉位置为三个第一管道211相互之间共同连通处,在交叉部位向上垂直连通第二管道212,第二管道212连通酶液储罐1的底部。Since the two chromatographic columns 21 located at the diagonal positions are communicated through the first pipelines 211, the six chromatographic columns 21 have three first pipelines 211, and the three first pipelines 211 are located on the same horizontal plane, There is a cross between the three first pipes 211, and the cross position is where the three first pipes 211 communicate with each other, and the second pipe 212 is vertically connected upward at the intersection, and the second pipe 212 is connected to the bottom of the enzyme liquid storage tank 1. .

液盘22(液盘22内的底部固定连接有一层圆形滤网,圆形滤网覆盖液盘22内的底面,圆形滤网的作用是过滤,防止堵塞微滤膜过滤装置31和纳滤膜过滤装置32,图中未画出圆形滤网)的底部中心连通有第三管道312,第三管道312连通在微滤膜过滤装置31的底部,微滤膜过滤装置31的顶部通过第五管道311连通纳滤膜过滤装置32的顶部,纳滤膜过滤装置32的底部通过第四管道321连通浓缩结晶装置4。The bottom of the liquid pan 22 (the bottom of the liquid pan 22 is fixedly connected with a layer of circular filter screen, the circular filter screen covers the bottom surface of the liquid pan 22, the function of the circular filter screen is to filter and prevent clogging of the microfiltration membrane filter device 31 and nanofiltration. The bottom center of the membrane filter device 32 (circular filter screen is not shown in the figure) is communicated with a third pipeline 312, the third pipeline 312 is connected to the bottom of the microfiltration membrane filter device 31, and the top of the microfiltration membrane filter device 31 passes through The fifth pipeline 311 communicates with the top of the nanofiltration membrane filtration device 32 , and the bottom of the nanofiltration membrane filtration device 32 communicates with the concentration and crystallization device 4 through the fourth pipeline 321 .

上述第一管道211、第二管道212、第三管道312、第四管道321,以及第五管道311均设置有阀门。The first pipe 211 , the second pipe 212 , the third pipe 312 , the fourth pipe 321 , and the fifth pipe 311 are all provided with valves.

实施例2分离提纯L-天冬氨酸的方法Embodiment 2 The method for separating and purifying L-aspartic acid

如图1-7所示,分离提纯L-天冬氨酸的方法,包括以下步骤:As shown in Figure 1-7, the method for separating and purifying L-aspartic acid includes the following steps:

S1、将50L,L-天冬氨酸浓度含量为160g/L的调节酶转化液泵入到酶液储罐1中,调节调节酶转化液的pH至4后,打开第二管道212上的阀门,调节酶转化液经第二管道212进入到第一管道211中,根据实际调节酶转化液的液量大小,选择打开第一管道211上的阀门个数,即选择通过层析柱21的个数。控制调节酶转化液流入层析柱21中的流速为100mL/min;S1, with 50L, the L-aspartic acid concentration content is that the regulating enzyme conversion liquid of 160g/L is pumped into the enzyme liquid storage tank 1, after the pH of the regulating enzyme conversion liquid is adjusted to 4, open the second pipeline 212 The valve is adjusted to enter the first pipeline 211 through the second pipeline 212, and the number of valves on the first pipeline 211 is selected to be opened according to the actual adjustment of the liquid volume of the enzymatic transformation solution, that is, the number of valves that pass through the chromatography column 21 is selected. number. Control and regulate the flow rate that the enzyme conversion solution flows into the chromatographic column 21 to be 100mL/min;

S2、吸附完毕,将氢氧化钠溶液泵入至酶液储罐1中,作为洗脱液,打开第二管道212上的阀门,以及层析柱21底部排液管上的阀门,氢氧化钠溶液带着L-天冬氨酸从层析柱21内分离,L-天冬氨酸洗脱液进入到液盘22中,控制氢氧化钠的洗脱流速为100mL/min;S2, the adsorption is completed, the sodium hydroxide solution is pumped into the enzyme liquid storage tank 1, as the eluent, open the valve on the second pipeline 212, and the valve on the drain pipe at the bottom of the chromatography column 21, sodium hydroxide The solution is separated from the chromatography column 21 with L-aspartic acid, and the L-aspartic acid eluate enters the liquid pan 22, and the elution flow rate of the controlled sodium hydroxide is 100 mL/min;

S3、洗脱过程中,打开第三管道312上的阀门,L-天冬氨酸洗脱液从第三管道312进入到微滤膜过滤装置31内,经微滤膜过滤装置31过滤后,从第五管道311进入到纳滤膜过滤装置32内,再从第四管道321进入到浓缩结晶装置4内进行减压浓缩;S3. During the elution process, open the valve on the third pipeline 312, and the L-aspartic acid eluate enters the microfiltration membrane filtration device 31 from the third pipeline 312, and after being filtered by the microfiltration membrane filtration device 31, Enter the nanofiltration membrane filtration device 32 from the fifth pipeline 311, and then enter the concentration and crystallization device 4 from the fourth pipeline 321 for decompression concentration;

S4、减压浓缩洗脱液后,加硫酸调浓缩液的pH值为1.5后,加入L-天冬氨酸晶种,进行结晶,经过滤、烘干后,得到L-天冬氨酸纯品。HPLC检测纯度为99.9%,收率91.6%。S4. After concentrating the eluent under reduced pressure, adding sulfuric acid to adjust the pH value of the concentrated solution to 1.5, adding L-aspartic acid seed crystals for crystallization, filtering and drying to obtain pure L-aspartic acid Taste. The purity detected by HPLC was 99.9%, and the yield was 91.6%.

L-天冬氨酸纯品的红外检测谱图如图8所示。The infrared detection spectrum of pure L-aspartic acid is shown in Figure 8.

实施例3分离提纯L-天冬氨酸的方法Embodiment 3 The method for separating and purifying L-aspartic acid

如图1--7所示,分离提纯L-天冬氨酸的方法,包括以下步骤:As shown in Figure 1--7, the method for separating and purifying L-aspartic acid includes the following steps:

S1、将50L,L-天冬氨酸浓度含量为210g/L的调节酶转化液泵入到酶液储罐1中,调节调节酶转化液的pH至8后,打开第二管道212上的阀门,调节酶转化液经第二管道212进入到第一管道211中,根据实际调节酶转化液的液量大小,选择打开第一管道211上的阀门个数,即选择通过层析柱21的个数。控制调节酶转化液流入层析柱21中的流速为2000mL/min;S1, with 50L, the L-aspartic acid concentration content is that the regulating enzyme conversion liquid of 210g/L is pumped into the enzyme liquid storage tank 1, after the pH of the regulating enzyme conversion liquid is adjusted to 8, open the second pipeline 212 The valve is adjusted to enter the first pipeline 211 through the second pipeline 212, and the number of valves on the first pipeline 211 is selected to be opened according to the actual adjustment of the liquid volume of the enzymatic transformation solution, that is, the number of valves that pass through the chromatography column 21 is selected. number. Control and regulate the flow rate that the enzyme conversion solution flows into the chromatography column 21 to be 2000mL/min;

S2、吸附完毕,将氢氧化钠溶液泵入至酶液储罐1中,作为洗脱液,打开第二管道212上的阀门以及,层析柱21底部排液管上的阀门,氢氧化钠溶液带着L-天冬氨酸从层析柱21内分离,L-天冬氨酸洗脱液进入到液盘22中,控制氢氧化钠的洗脱流速为500mL/min;S2, the adsorption is completed, the sodium hydroxide solution is pumped into the enzyme liquid storage tank 1, as the eluent, open the valve on the second pipeline 212 and the valve on the drain pipe at the bottom of the chromatography column 21, sodium hydroxide The solution is separated from the chromatography column 21 with L-aspartic acid, and the L-aspartic acid eluate enters the liquid pan 22, and the elution flow rate of the controlled sodium hydroxide is 500 mL/min;

S3、洗脱过程中,打开第三管道312上的阀门,L-天冬氨酸洗脱液从第三管道312进入到微滤膜过滤装置31内,经微滤膜过滤装置31过滤后,从第五管道311进入到纳滤膜过滤装置32内,再从第四管道321进入到浓缩结晶装置4内进行减压浓缩;S3. During the elution process, open the valve on the third pipeline 312, and the L-aspartic acid eluate enters the microfiltration membrane filtration device 31 from the third pipeline 312, and after being filtered by the microfiltration membrane filtration device 31, Enter the nanofiltration membrane filtration device 32 from the fifth pipeline 311, and then enter the concentration and crystallization device 4 from the fourth pipeline 321 for decompression concentration;

S4、减压浓缩洗脱液后,加硫酸调浓缩液的pH值为1.5后,加入L-天冬氨酸晶种,进行结晶,经过滤、烘干后,得到L-天冬氨酸纯品。HPLC检测纯度为99.9%,收率90.5%。S4. After concentrating the eluent under reduced pressure, adding sulfuric acid to adjust the pH value of the concentrated solution to 1.5, adding L-aspartic acid seed crystals for crystallization, filtering and drying to obtain pure L-aspartic acid Taste. The purity detected by HPLC was 99.9%, and the yield was 90.5%.

实施例4分离提纯L-天冬氨酸的方法Embodiment 4 The method for separating and purifying L-aspartic acid

如图1--7所示,分离提纯L-天冬氨酸的方法,包括以下步骤:As shown in Figure 1--7, the method for separating and purifying L-aspartic acid includes the following steps:

S1、将50L,L-天冬氨酸浓度含量为180g/L的调节酶转化液泵入到酶液储罐1中,调节调节酶转化液的pH至8后,打开第二管道212上的阀门,调节酶转化液经第二管道212进入到第一管道211中,根据实际调节酶转化液的液量大小,选择打开第一管道211上的阀门个数,即选择通过层析柱21的个数。控制调节酶转化液流入层析柱21中的流速为500mL/min;S1, with 50L, the L-aspartic acid concentration content is that the regulating enzyme transformation liquid of 180g/L is pumped into the enzyme liquid storage tank 1, after the pH of the regulation regulating enzyme transformation liquid is to 8, open the second pipeline 212 The valve is adjusted to enter the first pipeline 211 through the second pipeline 212, and the number of valves on the first pipeline 211 is selected to be opened according to the actual adjustment of the liquid volume of the enzymatic transformation solution, that is, the number of valves that pass through the chromatography column 21 is selected. number. The flow rate that the control and regulation enzyme conversion liquid flows into the chromatography column 21 is 500mL/min;

S2、吸附完毕,将氢氧化钠溶液泵入至酶液储罐1中,作为洗脱液,打开第二管道212上的阀门以及,层析柱21底部排液管上的阀门,氢氧化钠溶液带着L-天冬氨酸从层析柱21内分离,L-天冬氨酸洗脱液进入到液盘22中,控制氢氧化钠的洗脱流速为100mL/min;S2, the adsorption is completed, the sodium hydroxide solution is pumped into the enzyme liquid storage tank 1, as the eluent, open the valve on the second pipeline 212 and the valve on the drain pipe at the bottom of the chromatography column 21, sodium hydroxide The solution is separated from the chromatography column 21 with L-aspartic acid, and the L-aspartic acid eluate enters the liquid pan 22, and the elution flow rate of the controlled sodium hydroxide is 100 mL/min;

S3、洗脱过程中,打开第三管道312上的阀门,L-天冬氨酸洗脱液从第三管道312进入到微滤膜过滤装置31内,经微滤膜过滤装置31过滤后,从第五管道311进入到纳滤膜过滤装置32内,再从第四管道321进入到浓缩结晶装置4内进行减压浓缩;S3. During the elution process, open the valve on the third pipeline 312, and the L-aspartic acid eluate enters the microfiltration membrane filtration device 31 from the third pipeline 312, and after being filtered by the microfiltration membrane filtration device 31, Enter the nanofiltration membrane filtration device 32 from the fifth pipeline 311, and then enter the concentration and crystallization device 4 from the fourth pipeline 321 for decompression concentration;

S4、减压浓缩洗脱液后,加硫酸调浓缩液的pH值为2.8后,加入L-天冬氨酸晶种,进行结晶,经过滤、烘干后,得到L-天冬氨酸纯品。HPLC检测纯度为99.9%,收率90.3%。S4, after concentrating the eluent under reduced pressure, adding sulfuric acid to adjust the pH value of the concentrated solution to 2.8, adding L-aspartic acid seed crystals, carrying out crystallization, filtering and drying to obtain pure L-aspartic acid Taste. The purity detected by HPLC was 99.9%, and the yield was 90.3%.

实施例5分离提纯L-天冬氨酸的方法Embodiment 5 The method for separating and purifying L-aspartic acid

如图1--7所示,分离提纯L-天冬氨酸的方法,包括以下步骤:As shown in Figure 1--7, the method for separating and purifying L-aspartic acid includes the following steps:

S1、将50L,L-天冬氨酸浓度含量为200g/L的调节酶转化液泵入到酶液储罐1中,调节调节酶转化液的pH至6后,打开第二管道212上的阀门,调节酶转化液经第二管道212进入到第一管道211中,根据实际调节酶转化液的液量大小,选择打开第一管道211上的阀门个数,即选择通过层析柱21的个数。控制调节酶转化液流入层析柱21中的流速为100mL/min;S1, with 50L, the L-aspartic acid concentration content is that the regulating enzyme conversion liquid of 200g/L is pumped into the enzyme liquid storage tank 1, after adjusting the pH of the regulating enzyme conversion liquid to 6, open the second pipeline 212 The valve is adjusted to enter the first pipeline 211 through the second pipeline 212, and the number of valves on the first pipeline 211 is selected to be opened according to the actual adjustment of the liquid volume of the enzymatic transformation solution, that is, the number of valves that pass through the chromatography column 21 is selected. number. Control and regulate the flow rate that the enzyme conversion solution flows into the chromatographic column 21 to be 100mL/min;

S2、吸附完毕,将氢氧化钠溶液泵入至酶液储罐1中,作为洗脱液,打开第二管道212上的阀门以及,层析柱21底部排液管上的阀门,氢氧化钠溶液带着L-天冬氨酸从层析柱21内分离,L-天冬氨酸洗脱液进入到液盘22中,控制氢氧化钠的洗脱流速为500mL/min;S2, the adsorption is completed, the sodium hydroxide solution is pumped into the enzyme liquid storage tank 1, as the eluent, open the valve on the second pipeline 212 and the valve on the drain pipe at the bottom of the chromatography column 21, sodium hydroxide The solution is separated from the chromatography column 21 with L-aspartic acid, and the L-aspartic acid eluate enters the liquid pan 22, and the elution flow rate of the controlled sodium hydroxide is 500 mL/min;

S3、洗脱过程中,打开第三管道312上的阀门,L-天冬氨酸洗脱液从第三管道312进入到微滤膜过滤装置31内,经微滤膜过滤装置31过滤后,从第五管道311进入到纳滤膜过滤装置32内,再从第四管道321进入到浓缩结晶装置4内进行减压浓缩;S3. During the elution process, open the valve on the third pipeline 312, and the L-aspartic acid eluate enters the microfiltration membrane filtration device 31 from the third pipeline 312, and after being filtered by the microfiltration membrane filtration device 31, Enter the nanofiltration membrane filtration device 32 from the fifth pipeline 311, and then enter the concentration and crystallization device 4 from the fourth pipeline 321 for decompression concentration;

S4、减压浓缩洗脱液后,加硫酸调浓缩液的pH值为3.0后,加入L-天冬氨酸晶种,进行结晶,经过滤、烘干后,得到L-天冬氨酸纯品。HPLC检测纯度为99.9%,收率92.7%。S4. After concentrating the eluent under reduced pressure, adding sulfuric acid to adjust the pH value of the concentrated solution to 3.0, adding L-aspartic acid seed crystals for crystallization, filtering and drying to obtain pure L-aspartic acid Taste. The purity detected by HPLC was 99.9%, and the yield was 92.7%.

以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。The above descriptions are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent replacements and improvements made within the spirit and principles of the present invention shall be included in the protection of the present invention. within the range.

Claims (10)

1.一种L-天冬氨酸分离提纯装置,其特征在于,包括酶液储罐,所述酶液储罐连通有柱层析分离装置,所述柱层析分离装置连通有滤膜过滤装置,所述滤膜过滤装置连通有浓缩结晶装置;1. a L-aspartic acid separation and purification device, is characterized in that, comprises enzyme liquid storage tank, described enzyme liquid storage tank is communicated with column chromatography separation device, and described column chromatography separation device is communicated with membrane filtration device, the membrane filtration device is communicated with a concentration and crystallization device; 所述柱层析分离装置包括液盘,所述液盘的顶部连通有若干个层析柱,所述层析柱之间连通有第一管道,所述第一管道连通有第二管道,所述第二管道连通酶液储罐;The column chromatography separation device includes a liquid pan, the top of the liquid pan is connected with a plurality of chromatography columns, a first pipeline is connected between the chromatography columns, and the first pipeline is connected with a second pipeline, so the The second pipeline is communicated with the enzyme liquid storage tank; 所述液盘的底部连通有第三管道,所述第三管道连通滤膜过滤装置,所述滤膜过滤装置连通浓缩结晶装置;The bottom of the liquid pan is connected with a third pipeline, the third pipeline is connected with a membrane filtration device, and the membrane filtration device is connected with a concentration and crystallization device; 所述滤膜过滤装置包括微滤膜过滤装置和纳滤膜过滤装置,所述纳滤膜过滤装置的顶部和微滤膜过滤装置的顶部通过第五管道连通;The membrane filtration device includes a microfiltration membrane filtration device and a nanofiltration membrane filtration device, and the top of the nanofiltration membrane filtration device and the top of the microfiltration membrane filtration device are communicated through a fifth pipeline; 所述微滤膜过滤装置的底部连通第三管道,所述纳滤膜过滤装置的底部通过第四管道连通浓缩结晶装置;The bottom of the microfiltration membrane filtration device is communicated with the third pipeline, and the bottom of the nanofiltration membrane filtration device is communicated with the concentration and crystallization device through the fourth pipeline; 所述第一管道、第二管道、第三管道、第四管道,以及第五管道均设置有阀门。The first pipeline, the second pipeline, the third pipeline, the fourth pipeline, and the fifth pipeline are all provided with valves. 2.根据权利要求1所述的L-天冬氨酸分离提纯装置,其特征在于,所述液盘的顶部对称分布有6个层析柱,所述层析柱以液盘的盘心为对称中心,对称分布在液盘底部的侧边位置;2. L-aspartic acid separation and purification device according to claim 1, is characterized in that, the top of described liquid pan is symmetrically distributed with 6 chromatographic columns, and described chromatographic column takes the disk center of liquid pan as Symmetrical center, symmetrically distributed on the side of the bottom of the liquid pan; 位于对角位置处的所述层析柱之间通过第一管道连通,所述第一管道之间相互贯穿连通,所述第一管道的贯穿处向上垂直连通第二管道。The chromatographic columns located at the diagonal positions are communicated with each other through first pipes, the first pipes are in penetrating communication with each other, and the penetrating parts of the first pipes are vertically connected to the second pipes upward. 3.根据权利要求1所述的L-天冬氨酸分离提纯装置,其特征在于,所述第一管道两端的端部分别贯穿对应层析柱的顶部,所述第一管道的端部两端的端部分别连通有金属过滤球。3. L-aspartic acid separation and purification device according to claim 1, is characterized in that, the end of described first pipeline two ends penetrates the top of corresponding chromatography column respectively, and the end of described first pipeline is two The ends of the ends are respectively connected with metal filter balls. 4.根据权利要求3所述的L-天冬氨酸分离提纯装置,其特征在于,所述层析柱包括顶盖、底盖以及柱体,所述顶盖连接柱体的顶部,底盖连接柱体的底部,所述顶盖内设置有内腔,所述金属过滤球位于顶盖的内腔中,所述柱体内设置有层析空腔,所述层析空腔连通顶盖的内腔,所述层析空腔的腔顶位置连接有防冲击盘;4. L-aspartic acid separation and purification device according to claim 3, is characterized in that, described chromatographic column comprises top cover, bottom cover and cylinder, described top cover connects the top of cylinder, bottom cover The bottom of the column is connected, the top cover is provided with an inner cavity, the metal filter ball is located in the inner cavity of the top cover, the column is provided with a chromatography cavity, and the chromatography cavity is connected to the top cover. an inner cavity, an anti-shock disk is connected to the cavity top position of the chromatography cavity; 所述防冲击盘上开设有若干个通孔,所述通孔连通层析空腔,所述通孔上固定连接有滤网;A plurality of through holes are opened on the anti-shock disk, the through holes are connected to the chromatography cavity, and a filter screen is fixedly connected to the through holes; 所述底盖内设置有内腔,所述底盖的内腔连通层析空腔,所述底盖通过排液管连通在液盘的顶部,所述排液管设置有阀门。The bottom cover is provided with an inner cavity, the inner cavity of the bottom cover communicates with the chromatography cavity, and the bottom cover is communicated with the top of the liquid pan through a liquid drain pipe, and the liquid drain pipe is provided with a valve. 5.根据权利要求4所述的L-天冬氨酸分离提纯装置,其特征在于,所述层析空腔填充有离子交换树脂。5 . The L-aspartic acid separation and purification device according to claim 4 , wherein the chromatographic cavity is filled with ion exchange resin. 6 . 6.根据权利要求1所述的L-天冬氨酸分离提纯装置,其特征在于,所述浓缩结晶装置包括浓缩结晶釜,所述浓缩结晶釜内设置有搅拌装置,所述浓缩结晶釜连通有真空装置。6. L-aspartic acid separation and purification device according to claim 1, is characterized in that, described concentrated crystallization device comprises concentrated crystallization still, is provided with stirring device in described concentrated crystallization still, and described concentrated crystallization still communicates with There is a vacuum device. 7.根据权利要求1所述的L-天冬氨酸分离提纯装置,其特征在于,所述液盘内部中空,所述液盘的侧壁上设置有玻璃观察区。7 . The L-aspartic acid separation and purification device according to claim 1 , wherein the inside of the liquid pan is hollow, and a glass observation area is provided on the side wall of the liquid pan. 8 . 8.根据权利要求7所述的L-天冬氨酸分离提纯装置,其特征在于,所述玻璃观察区上设有刻度标线。8 . The L-aspartic acid separation and purification device according to claim 7 , wherein a scale mark is provided on the glass observation area. 9 . 9.根据权利要求8所述的L-天冬氨酸分离提纯装置,其特征在于,所述液盘内的底部固定连接有一层圆形滤网,所述圆形滤网覆盖液盘内的底面。9. L-aspartic acid separation and purification device according to claim 8, is characterized in that, the bottom in the described liquid pan is fixedly connected with a layer of circular filter screen, and the described circular filter screen covers the underside. 10.一种采用如权利要求1-9任意一项所述L-天冬氨酸分离提纯装置分离提纯L-天冬氨酸的方法,其特征在于,包括以下步骤:10. a method for adopting L-aspartic acid separation and purification device as described in any one of claims 1-9 to separate and purify L-aspartic acid, is characterized in that, comprises the following steps: S1、将50 L,L-天冬氨酸浓度含量为160-210g/L的调节酶转化液泵入到酶液储罐中,调节调节酶转化液的pH至4-8后,打开阀门,将调节酶转化液加入至柱层析分离装置中吸附,L-天冬氨酸吸附在柱层析分离装置中,控制调节酶转化液流入柱层析分离装置中的流速为100-2000mL/min;S1, pump 50 L, the L-aspartic acid concentration content is 160-210g/L regulating enzyme transformation liquid into the enzyme liquid storage tank, after adjusting the pH of regulating enzyme transformation liquid to 4-8, open the valve, Add the regulating enzyme conversion solution to the column chromatography separation device for adsorption, L-aspartic acid is adsorbed in the column chromatography separation device, and control the flow rate of the regulating enzyme conversion solution flowing into the column chromatography separation device to be 100-2000mL/min ; S2、吸附完毕,将氢氧化钠溶液泵入至酶液储罐中,作为洗脱液,打开阀门,利用氢氧化钠洗脱柱层析分离装置中吸附的L-天冬氨酸,控制氢氧化钠的洗脱流速为100-2000mL/min;S2. After the adsorption is completed, the sodium hydroxide solution is pumped into the enzyme liquid storage tank, and as the eluent, the valve is opened, and the L-aspartic acid adsorbed in the column chromatography separation device is eluted with sodium hydroxide to control the hydrogen The elution flow rate of sodium oxide is 100-2000mL/min; S3、洗脱过程中,打开阀门,洗脱液依次进入微滤膜过滤装置和纳滤膜过滤装置过滤后,进入浓缩结晶装置内;S3. During the elution process, open the valve, and the eluent enters the microfiltration membrane filtration device and the nanofiltration membrane filtration device in turn, and then enters the concentrated crystallization device; S4、减压浓缩洗脱液后,加硫酸调浓缩液的pH值为1.5-3.0后,加入L-天冬氨酸晶种,进行结晶,经过滤、烘干后,得到L-天冬氨酸纯品。S4, after concentrating the eluent under reduced pressure, adding sulfuric acid to adjust the pH value of the concentrated solution to 1.5-3.0, adding L-aspartic acid seed crystals to crystallize, and after filtering and drying to obtain L-aspartic acid Pure acid.
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