阅读说明：本技术 一种离子交换自动化控制装置及控制方法和控制系统 (Ion exchange automation control device, control method and control system ) 是由 张虓 李寿禧 梁凯 于 2021-04-01 设计创作，主要内容包括：本发明涉及一种离子交换自动化控制装置及控制方法和控制系统,离子交换柱的顶端设有酸类进料管道、常规进料管道和反顶液出料管道,离子交换柱的底端设有底部开口,稀盐酸管道和稀硫酸管道分别与酸类进料管道连通连接,纯化水管道和提取液管道分别与常规进料管道连通连接,稀液碱管道、解析液管道、排污管道和高氨氮排污管道分别与底部开口连通连接,反顶液管道与反顶液出料管道连通连接。工艺过程控制实现自动进料并计量,正反向自动洗涤实现离子交换柱的再生后纯化分离,自动上柱吸附,并通过在线分析仪分析实现提取液的馏分分离和收集,不需要操作人员在现场频繁操作,自动化程度高。(The invention relates to an ion exchange automatic control device, a control method and a control system, wherein an acid feed pipeline, a conventional feed pipeline and an anti-topping liquid discharge pipeline are arranged at the top end of an ion exchange column, a bottom opening is arranged at the bottom end of the ion exchange column, a dilute hydrochloric acid pipeline and a dilute sulfuric acid pipeline are respectively communicated and connected with the acid feed pipeline, a purified water pipeline and an extracting solution pipeline are respectively communicated and connected with the conventional feed pipeline, a dilute liquid alkali pipeline, a resolving solution pipeline, a blowdown pipeline and a high ammonia nitrogen blowdown pipeline are respectively communicated and connected with the bottom opening, and the anti-topping liquid pipeline is communicated and connected with the anti-topping liquid discharge pipeline. The process control realizes automatic feeding and metering, positive and negative automatic washing realizes the purification and separation after the regeneration of the ion exchange column, automatic column loading adsorption, and the separation and collection of the fraction of the extracting solution are realized through the analysis of an online analyzer, the frequent operation of operators on site is not needed, and the automation degree is high.)

1. The utility model provides an ion exchange automated control device, its characterized in that, includes ion exchange column (100), dilute hydrochloric acid pipeline (1), dilute sulphuric acid pipeline (2), dilute liquid alkali pipeline (3), purified water pipeline (4), extract pipeline (5), anti-top liquid pipeline (6), analytic liquid pipeline (7), sewage pipes (8) and high ammonia nitrogen sewage pipes (9), the top of ion exchange column (100) is equipped with sour feed tube way, conventional feed tube way and anti-top liquid ejection of compact pipeline, the bottom of ion exchange column (100) is equipped with the bottom opening, dilute hydrochloric acid pipeline (1) and dilute sulphuric acid pipeline (2) are connected with sour feed tube way intercommunication respectively, purified water pipeline (4) and extract pipeline (5) are connected with conventional feed tube way intercommunication respectively, dilute liquid alkali pipeline (3), analytic liquid pipeline (7), The sewage discharge pipeline (8) and the high ammonia nitrogen sewage discharge pipeline (9) are respectively communicated and connected with the bottom opening, and the reverse ejection liquid pipeline (6) is communicated and connected with the reverse ejection liquid discharge pipeline.

2. The automatic ion exchange control device according to claim 1, wherein a dilute hydrochloric acid flow meter (10) and a dilute hydrochloric acid feed on-off valve (15) are arranged on the dilute hydrochloric acid pipeline (1), a dilute sulfuric acid flow meter (11) and a dilute sulfuric acid feed on-off valve (16) are arranged on the dilute sulfuric acid pipeline (2), and a conventional feed adjusting valve (21) is arranged on a pipeline connecting the dilute hydrochloric acid pipeline (1) and the dilute sulfuric acid pipeline (2) with a conventional feed pipeline;

be equipped with purified water flowmeter (13) and purified water feed switch valve (18) on purified water pipeline (4), be equipped with extract flowmeter (14) and extract feed switch valve (19) on extract pipeline (5), be equipped with acid feed governing valve (20) on purified water pipeline (4) and extract pipeline (5) and the pipeline of acid charge pipeline connection.

3. The automatic ion exchange control device according to claim 2, characterized in that the conventional feed pipe is provided with a conventional feed switch valve (22) of the ion exchange column, and the acid feed pipe is provided with an acid feed switch valve (23) of the ion exchange column.

4. The automatic ion exchange control device according to claim 3, characterized in that a dilute caustic soda flow meter (12) and a dilute caustic soda feed switch valve (17) are arranged on the dilute caustic soda pipeline (3), the dilute caustic soda pipeline (3) is communicated and connected with the bottom opening through a conventional feed regulating valve (21), an anti-topping liquid feed switch valve (26) is arranged on a pipeline between the conventional feed regulating valve (21) and the bottom opening, and an ion exchange column emptying switch valve (24) and an anti-topping liquid discharge switch valve (25) are arranged on the anti-topping liquid discharge pipeline.

5. The automatic ion exchange control device according to claim 4, wherein a desorption liquid switch valve (27) and an online analyzer (37) are arranged on the desorption liquid pipeline (7), a blowdown switch valve (28) and a blowdown bypass switch valve (29) are arranged on the blowdown pipeline (8) in parallel, a pH transmitter (36) is arranged on the blowdown bypass switch valve (29), and a high ammonia nitrogen blowdown switch valve (30) is arranged on the high ammonia nitrogen blowdown pipeline (9).

6. The automatic control device for ion exchange according to claim 5, characterized in that the ion exchange column (100) is provided with an ion exchange column pressure transmitter (34) and an ion exchange column level gauge (35) on the side wall.

7. The automatic ion exchange control device according to claim 6, further comprising a first distillation tank (200), a second distillation tank (300) and a third distillation tank (400) which are respectively connected with the analysis liquid pipeline (7) in a communication manner, wherein the first distillation tank (200) is provided with a first distillation tank analysis liquid feeding switch valve (31), the second distillation tank (300) is provided with a second distillation tank analysis liquid feeding switch valve (32), and the third distillation tank (400) is provided with a third distillation tank analysis liquid feeding switch valve (33).

8. The control method of an ion exchange automation control device according to any one of claims 1 to 7, characterized in that the control method includes a regeneration process of the ion exchange column (100) and an upper column adsorption and fraction collection process of the ion exchange column (100), the regeneration process of the ion exchange column (100) includes the steps of:

step one, first water washing: automatically opening a purified water feeding switch valve (18), an ion exchange column conventional feeding switch valve (22) and a pollution discharge switch valve (28), adjusting the opening of a conventional feeding adjusting valve (21) to set flow for washing, and controlling the pressure of an ion exchange column pressure transmitter (34) and the liquid level of an ion exchange column liquid level meter (35); after the purified water flow meter (13) reaches the set volume, automatically closing the purified water feeding switch valve (18), the conventional ion exchange column feeding switch valve (22), the blowdown switch valve (28) and the conventional feeding adjusting valve (21);

step two, acid washing: automatically opening a dilute hydrochloric acid feeding switch valve (15), an ion exchange column acid feeding switch valve (23) and a blowdown switch valve (28), adjusting the opening of an acid feeding adjusting valve (20), adjusting to a set flow for pickling, and controlling the pressure of an ion exchange column pressure transmitter (34) and the liquid level of an ion exchange column liquid level meter (35); after the dilute hydrochloric acid flow meter (10) reaches a set volume, automatically closing the hydrochloric acid feeding switch valve (15), the ion exchange column acid type feeding switch valve (23), the blowdown switch valve (28) and the acid type feeding adjusting valve (20);

step three, second water washing: automatically opening a purified water feeding switch valve (18), an ion exchange column conventional feeding switch valve (22) and a pollution discharge switch valve (28), adjusting the opening of a conventional feeding adjusting valve (21) to set flow for washing, and controlling the pressure of an ion exchange column pressure transmitter (34) and the liquid level of an ion exchange column liquid level meter (35); after the purified water flow meter (13) reaches a set volume, a sewage bypass switch valve (29) is opened, a sewage switch valve (28) is closed, a pH transmitter (36) displays the pH value of the water washing on line, and when the pH value reaches a set value, a purified water feeding switch valve (18), an ion exchange column conventional feeding switch valve (22), the sewage bypass switch valve (29) and a conventional feeding adjusting valve (21) are closed;

fourthly, reverse alkali washing: automatically opening a dilute caustic soda feeding switch valve (17), an anti-topping liquid feeding switch valve (26) and an anti-topping liquid discharging switch valve (25), adjusting the opening of a conventional feeding adjusting valve (21) to set flow caustic washing, and controlling the pressure of an ion exchange column pressure transmitter (34); after the dilute caustic soda flow meter (12) reaches a set volume, closing the dilute caustic soda feeding switch valve (17), the reverse topping liquid feeding switch valve (26), the reverse topping liquid discharging switch valve (25) and the conventional feeding regulating valve (21);

fifthly, as in the third step, soaking the treated ion exchange column (100) for later use;

the upper column adsorption and fraction collection process of the ion exchange column (100) comprises the following steps:

sixthly, column loading and adsorption: automatically opening an extracting solution feeding switch valve (19), an ion exchange column conventional feeding switch valve (22) and a high ammonia nitrogen pollution discharge switch valve (30), adjusting the opening of a conventional feeding adjusting valve (21) to a set flow, loading the column for adsorption and separation, and controlling the pressure of an ion exchange column pressure transmitter (34) and the liquid level of an ion exchange column liquid level meter (35); after the extracting solution flow meter (14) reaches the set volume, closing the extracting solution feeding switch valve (19), the conventional ion exchange column feeding switch valve (22) and the conventional feeding regulating valve (21);

step seven, third water washing: automatically opening a purified water feeding switch valve (18) and an ion exchange column conventional feeding switch valve (22), adjusting the opening of a conventional feeding adjusting valve (21) to a set flow, washing, and controlling the pressure of an ion exchange column pressure transmitter (34) and an ion exchange column liquid level meter (35); after the purified water flow meter (13) reaches the primary set volume, a blowdown switch valve (28) is opened, and a high ammonia nitrogen blowdown switch valve (30) is closed; when the water is continuously washed to the secondary set volume, automatically closing the purified water feeding switch valve (18), the conventional ion exchange column feeding switch valve (22) and the conventional feeding adjusting valve (21);

eighth step, analysis: automatically opening a dilute sulfuric acid feeding switch valve (16), an ion exchange column acid feeding switch valve (23) and a solution switch valve (27), adjusting the opening of an acid feeding adjusting valve (20), adjusting to set flow analysis, and controlling the pressure of an ion exchange column pressure transmitter (34) and an ion exchange column liquid level meter (35); after the dilute sulfuric acid flow meter (11) reaches the set volume, automatically closing the blowdown switch valve (28) and starting fraction collection;

ninth, fraction collection: the on-line analyzer (37) opens a first fraction tank analysis liquid feeding switch valve (31), a second fraction tank analysis liquid feeding switch valve (32) and a third fraction tank analysis liquid feeding switch valve (33) according to the analysis numerical value, and the analysis liquid enters a first fraction tank (200), a second fraction tank (300) and a third fraction tank (400) respectively for collection so as to be used in the next process; after the collection is finished, closing a first fraction tank analysis liquid feeding switch valve (31), a second fraction tank analysis liquid feeding switch valve (32) and a third fraction tank analysis liquid feeding switch valve (33); and closing the dilute sulfuric acid feeding switch valve (16), the ion exchange column acid feeding switch valve (23) and the resolving liquid switch valve (27) for the next circulation.

9. The control system of the ion exchange automation control method according to claim 8, characterized in that the control system comprises:

the water washing unit is used for obtaining an instruction of entering a water washing step, and sending a closing instruction when the purified water flow meter (13) reaches a set amount and/or the pH transmitter (36) reaches a set pH value so as to close the purified water feeding switch valve (18), the conventional ion exchange column feeding switch valve (22), the conventional feeding adjusting valve (21) and the sewage discharge switch valve (28) or the sewage discharge bypass switch valve (29), and the control system prompts the completion of water washing;

the acid cleaning unit is used for obtaining an instruction for entering an acid cleaning step and sending a closing instruction when the dilute hydrochloric acid flow meter (10) reaches a set amount so as to close the hydrochloric acid feeding switch valve (15), the ion exchange column acid feeding switch valve (23), the pollution discharge switch valve (28) and the acid feeding adjusting valve (20), and the control system prompts the completion of acid cleaning;

the alkali washing unit is used for obtaining an instruction for entering an alkali washing step, and sending a closing instruction when a dilute caustic soda flowmeter (12) reaches a set amount so as to close a dilute caustic soda feeding switch valve (17), an anti-topping liquid feeding switch valve (26), an anti-topping liquid discharging switch valve (25) and a conventional feeding adjusting valve (21), and the control system prompts the completion of alkali washing;

the upper column adsorption unit is used for acquiring an instruction for entering the upper column adsorption step and sending a closing instruction when the extracting solution flowmeter (14) reaches a set amount so as to close the extracting solution feeding switch valve (19), the conventional ion exchange column feeding switch valve (22) and the conventional feeding adjusting valve (21), and the control system prompts the completion of upper column adsorption;

the analyzing unit is used for acquiring an instruction for entering the analyzing step and sending a closing instruction when the dilute sulfuric acid flow meter (11) reaches a set amount so as to close the pollution discharge switch valve (28), and the control system prompts the completion of the analysis;

and the fraction collection unit is used for acquiring an instruction entering a fraction collection step, sending an opening and closing instruction when an online analyzer (37) reaches a set amount so as to open and close a first fraction tank analysis liquid feeding switch valve (31), a second fraction tank analysis liquid feeding switch valve (32) and a third fraction tank analysis liquid feeding switch valve (33), stopping fraction collection when the set amount is reached, closing a dilute sulfuric acid feeding switch valve (16), an ion exchange column acid feeding switch valve (23) and an analysis liquid switch valve (27), and prompting the completion of fraction collection by a control system.

Technical Field

The invention relates to the technical field of biological medicines or foods, in particular to an ion exchange automation control device, a control method and a control system.

Background

The existing ion exchange process relates to multiple steps of water washing, acid washing, alkali washing, column adsorption, analysis, fraction collection and the like, wherein each step needs to manually open a corresponding valve and adjust the opening of the valve to control the flow and pressure; the flow and pressure of cleaning, upper column adsorption and desorption are different, and the feeding modes of alkaline cleaning and water cleaning are from top to bottom and from bottom to top. An operator is required to frequently and manually open, close and adjust the valve according to the process steps; particularly, in the adsorption process of the upper column, the volume of the upper column needs to be manually observed and recorded, and if the distance between the storage tank and the ion exchange column is long, a person needs to confirm the volume back and forth; not only the workload is large, but also the working efficiency is not high; especially, make mistakes more easily when the night work, increase misoperation's risk. More importantly, once the valve is opened wrongly, the raw materials and the products are lost, so that the process yield is reduced and the environmental protection treatment cost is increased.

Therefore, it is necessary to provide an automatic control device, a control method and a control system for ion exchange, which can realize the automatic continuous separation operation of the ion exchange unit through the control of the instruments and valves.

Disclosure of Invention

In view of the above, the present invention provides an automatic control device, a control method and a control system for ion exchange, which realize automatic continuous regeneration of an ion exchange column and collection cycle of fraction adsorbed on the column through arrangement of pipelines and valves.

In order to solve the technical problems, the invention adopts the following technical scheme:

the utility model provides an ion exchange automated control device, includes ion exchange column, dilute hydrochloric acid pipeline, dilute sulphuric acid pipeline, dilute caustic soda pipeline, purified water pipeline, extract pipeline, anti-apical liquid pipeline, analytic liquid pipeline, sewage pipes and high ammonia nitrogen sewage pipes, the top of ion exchange column is equipped with sour feed line, conventional feed line and anti-apical liquid ejection of compact pipeline, the bottom of ion exchange column is equipped with the bottom opening, dilute hydrochloric acid pipeline and dilute sulphuric acid pipeline are connected with sour feed line intercommunication respectively, purified water pipeline and extract pipeline are connected with conventional feed line intercommunication respectively, dilute caustic soda pipeline, analytic liquid pipeline, sewage pipes and high ammonia nitrogen sewage pipes are connected with bottom opening intercommunication respectively, anti-apical liquid pipeline is connected with anti-apical liquid ejection of compact pipeline intercommunication.

Preferably, a dilute hydrochloric acid flow meter and a dilute hydrochloric acid feeding switch valve are arranged on the dilute hydrochloric acid pipeline, a dilute sulfuric acid flow meter and a dilute sulfuric acid feeding switch valve are arranged on the dilute sulfuric acid pipeline, and a conventional feeding adjusting valve is arranged on a pipeline connecting the dilute hydrochloric acid pipeline and the dilute sulfuric acid pipeline with a conventional feeding pipeline; the purified water pipeline is provided with a purified water flow meter and a purified water feeding switch valve, the extracting solution pipeline is provided with an extracting solution flow meter and an extracting solution feeding switch valve, and the purified water pipeline and the extracting solution pipeline are provided with an acid feeding regulating valve on the pipeline connected with the acid feeding pipeline.

Preferably, the conventional feed pipeline is provided with an ion exchange column conventional feed switch valve, and the acid feed pipeline is provided with an ion exchange column acid feed switch valve.

Preferably, be equipped with dilute caustic soda flowmeter and dilute caustic soda feed ooff valve on the dilute caustic soda pipeline, dilute caustic soda pipeline is connected with bottom opening intercommunication through conventional feed governing valve, be equipped with anti-topping liquid feed ooff valve on the pipeline between conventional feed governing valve and the bottom opening, be equipped with ion exchange column unloading ooff valve and anti-topping liquid ejection of compact ooff valve on the anti-topping liquid ejection of compact pipeline.

Preferably, be equipped with analytic liquid ooff valve and on-line analyzer on the analytic liquid pipeline, parallelly connected blowdown on the sewage pipes switch valve and the blowdown bypass ooff valve of being equipped with, be equipped with the pH changer on the blowdown bypass ooff valve, be equipped with high ammonia nitrogen blowdown ooff valve on the high ammonia nitrogen sewage pipes.

Preferably, an ion exchange column pressure transmitter and an ion exchange column liquid level meter are arranged on the side wall of the ion exchange column.

Preferably, controlling means still includes first fraction jar, second fraction jar and third fraction jar with analysis liquid pipeline intercommunication connection respectively, be equipped with the analysis liquid feed switch valve of first fraction jar on the first fraction jar, be equipped with the analysis liquid feed switch valve of second fraction jar on the second fraction jar, be equipped with the analysis liquid feed switch valve of third fraction jar on the third fraction jar.

According to the control method of the ion exchange automation control device, the control method comprises a regeneration process of the ion exchange column and an upper column adsorption and fraction collection process of the ion exchange column, and the regeneration process of the ion exchange column comprises the following steps:

step one, first water washing: automatically opening a purified water feeding switch valve, an ion exchange column conventional feeding switch valve and a sewage discharge switch valve, adjusting the opening of a conventional feeding adjusting valve to a set flow, washing, and controlling the pressure of an ion exchange column pressure transmitter and the liquid level of an ion exchange column liquid level meter; and after the purified water flow meter reaches the set volume, automatically closing the purified water feeding switch valve, the conventional ion exchange column feeding switch valve, the pollution discharge switch valve and the conventional feeding adjusting valve. The first water washing is used for cleaning impurities on the surfaces and in the pores of the resin in the pipeline and the ion exchange column.

Step two, acid washing: automatically opening a dilute hydrochloric acid feeding switch valve, an ion exchange column acid feeding switch valve and a pollution discharge switch valve, adjusting the opening of an acid feeding adjusting valve to a set flow for pickling, and controlling the pressure of an ion exchange column pressure transmitter and the liquid level of an ion exchange column liquid level meter; and after the dilute hydrochloric acid flow meter reaches the set volume, automatically closing the hydrochloric acid feeding switch valve, the ion exchange column acid type feeding switch valve, the pollution discharge switch valve and the acid type feeding regulating valve. The acid wash serves to convert the resin to Cl^-And removing acid-soluble impurities.

Step three, second water washing: automatically opening a purified water feeding switch valve, an ion exchange column conventional feeding switch valve and a sewage discharge switch valve, adjusting the opening of a conventional feeding adjusting valve to a set flow, washing, and controlling the pressure of an ion exchange column pressure transmitter and the liquid level of an ion exchange column liquid level meter; and after the purified water flow meter reaches a set volume, opening the sewage discharge bypass switch valve, closing the sewage discharge switch valve, displaying the pH value of the washing water on line by the pH transmitter, and closing the purified water feeding switch valve, the conventional ion exchange column feeding switch valve, the sewage discharge bypass switch valve and the conventional feeding adjusting valve when the pH value reaches a set value. The second water washing is used for washing impurities on the surfaces and in pores of the resin in the pipeline and the ion exchange column and keeping the pH of the system neutral.

Fourthly, reverse alkali washing: automatically opening a dilute alkali liquid feeding switch valve, an anti-topping liquid feeding switch valve and an anti-topping liquid discharging switch valve, adjusting the opening of a conventional feeding adjusting valve to set flow alkali washing, and controlling the pressure of an ion exchange column pressure transmitter; and after the dilute caustic soda flow meter reaches the set volume, closing the dilute caustic soda feeding switch valve, the reverse topping liquid discharging switch valve and the conventional feeding regulating valve. The reverse alkali washing has the function of converting the resin into OH^-And removing alkali soluble impurities.

Step five, like the step three, soaking the treated ion exchange column for later use; the step has the functions of cleaning impurities on the surfaces and in pores of the resin in the pipeline and the ion exchange column, keeping the pH of the system neutral, keeping the resin in a wet state by soaking, preventing the resin from being dried to influence the exchange capacity and efficiency, and waiting for the adsorption on the column.

The upper column adsorption and fraction collection process of the ion exchange column comprises the following steps:

sixthly, column loading and adsorption: automatically opening an extracting solution feeding switch valve, an ion exchange column conventional feeding switch valve and a high ammonia nitrogen pollution discharge switch valve, adjusting the opening of a conventional feeding adjusting valve to a set flow, performing column adsorption separation, and controlling the pressure of an ion exchange column pressure transmitter and the liquid level of an ion exchange column liquid level meter; and after the extracting solution flow meter reaches the set volume, closing the extracting solution feeding switch valve, the conventional ion exchange column feeding switch valve and the conventional feeding adjusting valve. The function of the upper column adsorption is that the resin adsorbs effective components in the upper column extracting solution.

Step seven, third water washing: automatically opening a purified water feeding switch valve and an ion exchange column conventional feeding switch valve, adjusting the opening of a conventional feeding adjusting valve to a set flow, washing, and controlling the pressure of an ion exchange column pressure transmitter and a liquid level meter of the ion exchange column; after the purified water flow meter reaches the primary set volume, opening a blowdown switch valve, and closing a high ammonia nitrogen blowdown switch valve; and when the water is continuously washed to the secondary set volume, automatically closing the purified water feeding switch valve, the conventional ion exchange column feeding switch valve and the conventional feeding adjusting valve. The third water wash serves to clean the lines and remove impurities bound to the resin functionality in the ion exchange column.

Eighth step, analysis: automatically opening a dilute sulfuric acid feeding switch valve, an ion exchange column acid feeding switch valve and a resolving liquid switch valve, adjusting the opening of an acid feeding adjusting valve to set flow resolution, and controlling the pressure of an ion exchange column pressure transmitter and an ion exchange column liquid level meter; and after the dilute sulfuric acid flow meter reaches the set volume, automatically closing the pollution discharge switch valve and starting fraction collection. The desorption functions to elute effective components adsorbed by the resin by dilute sulfuric acid.

Ninth, fraction collection: the on-line analyzer starts a first fraction tank analytic liquid feeding switch valve, a second fraction tank analytic liquid feeding switch valve and a third fraction tank analytic liquid feeding switch valve according to the analysis numerical value, and the analytic liquid feeding switch valves respectively enter a first fraction tank, a second fraction tank and a third fraction tank to be collected for use in the next working procedure; after the collection is finished, closing the first fraction tank analysis liquid feeding switch valve, the second fraction tank analysis liquid feeding switch valve and the third fraction tank analysis liquid feeding switch valve; the dilute sulfuric acid feed on-off valve, ion exchange column acid feed on-off valve, and eluent on-off valve were closed for the next cycle. The fraction collection function is to collect different fractions according to the impurity distribution in the elution process and the result of the on-line analyzer.

The control system of the ion exchange automation control method comprises the following steps:

the water washing unit is used for obtaining an instruction for entering the water washing step, and sending a closing instruction when the purified water flow meter reaches a set amount and/or the pH transmitter reaches a set pH value so as to close the purified water feeding switch valve, the conventional ion exchange column feeding switch valve, the conventional feeding adjusting valve and the sewage discharge switch valve or the sewage discharge bypass switch valve, and the control system prompts the completion of water washing;

the acid cleaning unit is used for acquiring an instruction for entering the acid cleaning step and sending a closing instruction when the dilute hydrochloric acid flow meter reaches a set amount so as to close the hydrochloric acid feeding switch valve, the ion exchange column acid feeding switch valve, the pollution discharge switch valve and the acid feeding regulating valve, and the control system prompts the completion of acid cleaning;

the alkali washing unit is used for acquiring an instruction for entering an alkali washing step and sending a closing instruction when the dilute alkali liquid flow meter reaches a set amount so as to close the dilute alkali liquid feeding switch valve, the reverse top liquid discharging switch valve and the conventional feeding adjusting valve, and the control system prompts the completion of alkali washing;

the upper column adsorption unit is used for acquiring an instruction for entering the upper column adsorption step and sending a closing instruction when the extracting solution flowmeter reaches a set amount so as to close the extracting solution feeding switch valve, the conventional ion exchange column feeding switch valve and the conventional feeding adjusting valve, and the control system prompts the completion of upper column adsorption;

the analysis unit is used for acquiring an instruction for entering the analysis step and sending a closing instruction when the dilute sulfuric acid flow meter reaches a set amount so as to close the pollution discharge switch valve, and the control system prompts the completion of the analysis;

and the fraction collection unit is used for acquiring an instruction entering the fraction collection step, sending an opening and closing instruction when the online analyzer reaches a set amount so as to open and close the first fraction tank analysis liquid feeding switch valve, the second fraction tank analysis liquid feeding switch valve and the third fraction tank analysis liquid feeding switch valve, stopping fraction collection when the set amount is reached, closing the dilute sulfuric acid feeding switch valve, the ion exchange column acid feeding switch valve and the analysis liquid switch valve, and prompting the completion of fraction collection by the control system.

The invention has the following beneficial effects:

according to the automatic control device, the control method and the control system for the ion exchange, due to the adoption of the technical scheme, the technical process control realizes automatic feeding and metering, the forward and reverse automatic washing realizes the regeneration, purification and separation of the ion exchange column, the adsorption on the column is automatically realized, the fraction separation and collection of the extracting solution are realized through the analysis of the online analyzer, the frequent operation of operators on site is not needed, and the automation degree is high. Can be used in the field of extracting solution ion exchange separation and purification, in particular to the fields with more ion exchange columns and the environment with severe field operation environment.

The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical means of the present invention more clearly understood and to make the technical means implementable in accordance with the contents of the description, and to make the above and other objects, technical features, and advantages of the present invention more comprehensible, one or more preferred embodiments are described below in detail with reference to the accompanying drawings.

Drawings

One or more embodiments are illustrated by way of example in the accompanying drawings, which correspond to the figures in which like reference numerals refer to similar elements and which are not to scale unless otherwise specified.

Fig. 1 shows a schematic structural diagram of an ion exchange automation control device according to the present invention.

Description of the main reference numerals:

1-dilute hydrochloric acid pipeline, 2-dilute sulfuric acid pipeline, 3-dilute liquid alkali pipeline, 4-purified water pipeline, 5-extract liquid pipeline, 6-reverse top liquid pipeline, 7-analytic liquid pipeline, 8-sewage pipeline, 9-high ammonia nitrogen sewage pipeline, 10-dilute hydrochloric acid flowmeter, 11-dilute sulfuric acid flowmeter, 12-dilute liquid alkali flowmeter, 13-purified water flowmeter, 14-extract liquid flowmeter, 15-dilute hydrochloric acid feed switch valve, 16-dilute sulfuric acid feed switch valve, 17-dilute liquid alkali feed switch valve, 18-purified water feed switch valve, 19-extract liquid feed switch valve, 20-acid feed regulating valve, 21-conventional feed regulating valve, 22-ion exchange column conventional feed switch valve, 23-ion exchange column acid feed switch valve, 24-ion exchange column emptying switch valve, 25-reverse top liquid discharging switch valve, 26-reverse top liquid feeding switch valve, 27-analytic liquid switch valve, 28-blowdown switch valve, 29-blowdown bypass switch valve, 30-high ammonia nitrogen blowdown switch valve, 31-first fraction tank analytic liquid feeding switch valve, 32-second fraction tank analytic liquid feeding switch valve, 33-third fraction tank analytic liquid feeding switch valve, 34-ion exchange column pressure transmitter, 35-ion exchange column liquid level meter, 36-pH transmitter, 37-online analyzer, 100-ion exchange column, 200-first fraction tank, 300-second fraction tank and 400-third fraction tank.

Detailed Description

The following detailed description of the present invention is provided in conjunction with the accompanying drawings, but it should be understood that the scope of the present invention is not limited to the specific embodiments.

Throughout the specification and claims, unless explicitly stated otherwise, the word "comprise", or variations such as "comprises" or "comprising", will be understood to imply the inclusion of a stated element or component but not the exclusion of any other element or component.

Spatially relative terms, such as "below," "lower," "upper," "above," "upper," and the like, may be used herein for ease of description to describe one element or feature's relationship to another element or feature in the figures. It will be understood that the spatially relative terms are intended to encompass different orientations of the object in use or operation in addition to the orientation depicted in the figures. For example, if the items in the figures are turned over, elements described as "below" or "beneath" other elements or features would then be oriented "above" the elements or features. Thus, the exemplary term "below" can encompass both an orientation of below and above. The article may be otherwise oriented (rotated 90 degrees or at other orientations) and the spatially relative terms used herein should be interpreted accordingly.

As shown in figure 1, an automatic control device for ion exchange comprises an ion exchange column 100, a dilute hydrochloric acid pipeline 1, a dilute sulfuric acid pipeline 2, a dilute alkali solution pipeline 3, a purified water pipeline 4, an extracting solution pipeline 5, a reverse top solution pipeline 6, a resolving solution pipeline 7, a sewage pipeline 8 and a high ammonia nitrogen sewage pipeline 9, the top end of the ion exchange column 100 is provided with an acid feeding pipeline, a conventional feeding pipeline and a reverse top liquid discharging pipeline, the bottom end of the ion exchange column 100 is provided with a bottom opening, the dilute hydrochloric acid pipeline 1 and the dilute sulfuric acid pipeline 2 are respectively communicated and connected with an acid feeding pipeline, purified water pipeline 4 and extract pipeline 5 are connected with conventional charge-in pipeline intercommunication respectively, weak liquid alkali pipeline 3, analytic liquid pipeline 7, sewage pipes 8 and high ammonia nitrogen sewage pipes 9 are connected with bottom opening intercommunication respectively, anti-flowing back pipeline 6 is connected with anti-flowing back ejection of compact pipeline intercommunication.

A dilute hydrochloric acid flowmeter 10 and a dilute hydrochloric acid feeding switch valve 15 are arranged on the dilute hydrochloric acid pipeline 1, a dilute sulfuric acid flowmeter 11 and a dilute sulfuric acid feeding switch valve 16 are arranged on the dilute sulfuric acid pipeline 2, and a conventional feeding adjusting valve 21 is arranged on a pipeline connecting the dilute hydrochloric acid pipeline 1 and the dilute sulfuric acid pipeline 2 with a conventional feeding pipeline; the purified water pipeline 4 is provided with a purified water flow meter 13 and a purified water feeding switch valve 18, the extracting solution pipeline 5 is provided with an extracting solution flow meter 14 and an extracting solution feeding switch valve 19, and the pipelines of the purified water pipeline 4 and the extracting solution pipeline 5 connected with the acid feeding pipeline are provided with an acid feeding regulating valve 20.

And the conventional feeding pipeline is provided with an ion exchange column conventional feeding switch valve 22, and the acid feeding pipeline is provided with an ion exchange column acid feeding switch valve 23.

Be equipped with weak solution alkali flowmeter 12 and weak solution alkali feed switch valve 17 on the weak solution alkali pipeline 3, weak solution alkali pipeline 3 is connected with bottom opening intercommunication through conventional feed governing valve 21, be equipped with anti-top liquid feed switch valve 26 on the pipeline between conventional feed governing valve 21 and the bottom opening, be equipped with ion exchange column atmospheric switch valve 24 and anti-top liquid ejection of compact switch valve 25 on the anti-top liquid ejection of compact pipeline.

The analysis liquid pipeline 7 is provided with an analysis liquid switch valve 27 and an online analyzer 37, the sewage drain pipeline 8 is provided with a sewage drain switch valve 28 and a sewage drain bypass switch valve 29 in parallel, the sewage drain bypass switch valve 29 is provided with a pH transmitter 36, and the high ammonia nitrogen sewage drain pipeline 9 is provided with a high ammonia nitrogen sewage drain switch valve 30.

An ion exchange column pressure transmitter 34 and an ion exchange column liquid level meter 35 are arranged on the side wall of the ion exchange column 100.

The control device further comprises a first fraction tank 200, a second fraction tank 300 and a third fraction tank 400 which are respectively communicated with the analysis liquid pipeline 7, wherein the first fraction tank 200 is provided with a first fraction tank analysis liquid feeding switch valve 31, the second fraction tank 300 is provided with a second fraction tank analysis liquid feeding switch valve 32, and the third fraction tank 400 is provided with a third fraction tank analysis liquid feeding switch valve 33.

According to the control method of the ion exchange automation control device, the control method comprises the regeneration process of the ion exchange column 100 and the upper column adsorption and fraction collection process of the ion exchange column 100, the regeneration process of the ion exchange column 100 comprises the following steps:

step one, first water washing: automatically opening a purified water feeding switch valve 18, an ion exchange column conventional feeding switch valve 22 and a pollution discharge switch valve 28, adjusting the opening of a conventional feeding adjusting valve 21 to set flow for washing, and controlling the pressure of an ion exchange column pressure transmitter 34 and the liquid level of an ion exchange column liquid level meter 35; after the purified water flow meter 13 reaches the set volume, the purified water feed on-off valve 18, the ion exchange column normal feed on-off valve 22, the blowdown on-off valve 28, and the normal feed adjusting valve 21 are automatically closed. The first water wash serves to clean the lines and impurities in the resin surfaces and pores of the ion exchange column 100.

Step two, acid washing: automatically opening a dilute hydrochloric acid feeding switch valve 15, an ion exchange column acid feeding switch valve 23 and a blowdown switch valve 28, adjusting the opening of an acid feeding adjusting valve 20 to a set flow for pickling, and controlling the pressure of an ion exchange column pressure transmitter 34 and the liquid level of an ion exchange column liquid level meter 35; after the dilute hydrochloric acid flow meter 10 reaches the set volume, the hydrochloric acid feeding switch valve 15, the ion exchange column acid feeding switch valve 23, the blowdown switch valve 28 and the acid feeding adjusting valve 20 are automatically closed. The acid wash serves to convert the resin to Cl^-And removing acid-soluble impurities.

Step three, second water washing: automatically opening a purified water feeding switch valve 18, an ion exchange column conventional feeding switch valve 22 and a pollution discharge switch valve 28, adjusting the opening of a conventional feeding adjusting valve 21 to set flow for washing, and controlling the pressure of an ion exchange column pressure transmitter 34 and the liquid level of an ion exchange column liquid level meter 35; after the purified water flow meter 13 reaches the set volume, the blowdown bypass switch valve 29 is opened, the blowdown switch valve 28 is closed, the pH transmitter 36 displays the pH of the water washing on line, and when the pH reaches the set value, the purified water feed switch valve 18, the ion exchange column conventional feed switch valve 22, the blowdown bypass switch valve 29 and the conventional feed adjusting valve 21 are closed. The second water washing is used for cleaning impurities on the surface and in the pores of the resin in the pipeline and the ion exchange column 100 and keeping the pH of the system neutral.

Fourthly, reverse alkali washing: automatically opening a dilute alkali liquid feeding switch valve 17, an anti-topping liquid feeding switch valve 26 and an anti-topping liquid discharging switch valve 25, adjusting the opening of a conventional feeding adjusting valve 21 to set flow alkali washing, and controlling the pressure of an ion exchange column pressure transmitter 34; and after the dilute caustic soda flow meter 12 reaches the set volume, closing the dilute caustic soda feeding switch valve 17, the reverse topping liquid feeding switch valve 26, the reverse topping liquid discharging switch valve 25 and the conventional feeding regulating valve 21. The reverse alkali washing has the function of converting the resin into OH^-And removing alkali soluble impurities.

Step five, like the step three, soaking the treated ion exchange column 100 for later use; this step serves to clean the tubing and impurities in the resin surface and pores of the ion exchange column 100, maintain the pH of the system neutral, and soak to keep the resin wet, preventing the resin from drying out and affecting the exchange capacity and efficiency, waiting for adsorption on the column.

The upper column adsorption and fraction collection process of the ion exchange column 100 comprises the following steps:

sixthly, column loading and adsorption: automatically opening an extracting solution feeding switch valve 19, an ion exchange column conventional feeding switch valve 22 and a high ammonia nitrogen pollution discharge switch valve 30, adjusting the opening of a conventional feeding adjusting valve 21 to a set flow, performing column adsorption separation, and controlling the pressure of an ion exchange column pressure transmitter 34 and the liquid level of an ion exchange column liquid level meter 35; after the extract flow meter 14 reaches the set volume amount, the extract feed on-off valve 19, the ion exchange column normal feed on-off valve 22, and the normal feed adjusting valve 21 are closed. The function of the upper column adsorption is that the resin adsorbs effective components in the upper column extracting solution.

Step seven, third water washing: automatically opening a purified water feeding switch valve 18 and an ion exchange column conventional feeding switch valve 22, adjusting the opening of a conventional feeding adjusting valve 21 to a set flow, washing, and controlling the pressure of an ion exchange column pressure transmitter 34 and an ion exchange column liquid level meter 35; after the purified water flow meter 13 reaches the primary set volume, the blowdown on-off valve 28 is opened, and the high ammonia nitrogen blowdown on-off valve 30 is closed; and when the water washing is continued to the secondary set volume, automatically closing the purified water feeding switch valve 18, the ion exchange column conventional feeding switch valve 22 and the conventional feeding adjusting valve 21. The third water wash serves to clean the lines and remove impurities bound to the resin functionality in the ion exchange column 100.

Eighth step, analysis: automatically opening a dilute sulfuric acid feeding switch valve 16, an ion exchange column acid feeding switch valve 23 and a resolving liquid switch valve 27, adjusting the opening degree of an acid feeding adjusting valve 20 to set flow resolution, and controlling the pressure of an ion exchange column pressure transmitter 34 and an ion exchange column liquid level meter 35; after the dilute sulfuric acid flow meter 11 reaches the set volume, the blowdown on-off valve 28 is automatically closed, and fraction collection is started. The desorption functions to elute effective components adsorbed by the resin by dilute sulfuric acid.

Ninth, fraction collection: the on-line analyzer 37 opens the first fraction tank analysis liquid feeding switch valve 31, the second fraction tank analysis liquid feeding switch valve 32 and the third fraction tank analysis liquid feeding switch valve 33 according to the analysis numerical value, and the analysis liquid respectively enters the first fraction tank 200, the second fraction tank 300 and the third fraction tank 400 for collection so as to be used in the next process; after the collection is finished, closing the first fraction tank analysis liquid feeding switch valve 31, the second fraction tank analysis liquid feeding switch valve 32 and the third fraction tank analysis liquid feeding switch valve 33; the dilute sulfuric acid feed on-off valve 16, the ion exchange column acid feed on-off valve 23, and the resolving liquid on-off valve 27 are closed for the next cycle. The effect of fraction collection is to perform different fraction collections depending on the results of the on-line analyzer 37 depending on the elution process impurity profile.

The control system of the ion exchange automation control method comprises the following steps:

the water washing unit is used for acquiring an instruction of entering the water washing step, and sending a closing instruction when the purified water flow meter 13 reaches a set amount and/or the pH transmitter 36 reaches a set pH value so as to close the purified water feeding switch valve 18, the ion exchange column conventional feeding switch valve 22, the conventional feeding adjusting valve 21 and the sewage discharge switch valve 28 or the sewage discharge bypass switch valve 29, and the control system prompts the completion of water washing;

the acid cleaning unit is used for obtaining an instruction for entering the acid cleaning step and sending a closing instruction when the dilute hydrochloric acid flowmeter 10 reaches a set amount so as to close the hydrochloric acid feeding switch valve 15, the ion exchange column acid feeding switch valve 23, the pollution discharge switch valve 28 and the acid feeding adjusting valve 20, and the control system prompts the completion of acid cleaning;

the alkali washing unit is used for acquiring an instruction for entering an alkali washing step, and sending a closing instruction when the dilute caustic flowmeter 12 reaches a set amount so as to close the dilute caustic feeding switch valve 17, the reverse topping liquid feeding switch valve 26, the reverse topping liquid discharging switch valve 25 and the conventional feeding adjusting valve 21, and the control system prompts that the alkali washing is finished;

the upper column adsorption unit is used for acquiring an instruction for entering the upper column adsorption step and sending a closing instruction when the extracting solution flowmeter 14 reaches a set amount so as to close the extracting solution feeding switch valve 19, the conventional ion exchange column feeding switch valve 22 and the conventional feeding adjusting valve 21, and the control system prompts the completion of upper column adsorption;

the analysis unit is used for acquiring an instruction for entering the analysis step and sending a closing instruction when the dilute sulfuric acid flow meter 11 reaches a set amount so as to close the pollution discharge switch valve 28 and prompt the control system to finish the analysis;

and the fraction collection unit is used for acquiring an instruction entering a fraction collection step, sending an opening and closing instruction when the online analyzer 37 reaches a set amount so as to open and close the first fraction tank analysis liquid feeding switch valve 31, the second fraction tank analysis liquid feeding switch valve 32 and the third fraction tank analysis liquid feeding switch valve 33, stopping fraction collection when the set amount is reached, closing the dilute sulfuric acid feeding switch valve 16, the ion exchange column acid feeding switch valve 23 and the analysis liquid switch valve 27, and prompting the completion of fraction collection by the control system.

The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications as are suited to the particular use contemplated. Any simple modifications, equivalent changes and modifications made to the above exemplary embodiments shall fall within the scope of the present invention.