A kind of low-loss Amine Solutions purification device and its application method

文档序号:1747805 发布日期:2019-11-29 浏览:29次 中文

阅读说明:本技术 一种低损耗有机胺溶液净化装置及其使用方法 (A kind of low-loss Amine Solutions purification device and its application method ) 是由 王金意 郜时旺 刘练波 牛红伟 郭东方 汪世清 范旭 王孟 孙美琪 白国威 于 2019-09-19 设计创作,主要内容包括:本发明公开一种低损耗有机胺溶液净化装置及其使用方法,装置包括离子交换床,所述离子交换床的上端进料口通过管道安装有惰性气体气瓶、第五储液罐和第二加液泵,所述离子交换床的下端进料口通过管道连接有第一加液泵,所述第一加液泵的抽料口通过管道连接有第一储液罐;所述离子交换床的下端出料口通过管道连接有第二储液罐、第三储液罐和第四储液罐,所述离子交换床的下端出料管道安装有多重全反射红外光谱分析仪;所述离子交换床的上端出料口通过管道连接有第四储液罐。本发明便于工作人员通过多重全反射红外光谱分析仪D1实时检测结果控制阀门,避免了现有技术采用固化的运行程序对实际运行情况响应差,不能自主优化运行参数的缺点。(The present invention discloses a kind of low-loss Amine Solutions purification device and its application method, device includes ion exchange bed, the upper end feed inlet of the ion exchange bed has inert gas gas cylinder, the 5th fluid reservoir and the second fluid filling pump by Pipe installing, the lower end feed inlet of the ion exchange bed is connected with the first fluid filling pump by pipeline, and the extraction opening of first fluid filling pump is connected with the first fluid reservoir by pipeline;The lower end discharge port of the ion exchange bed is connected with the second fluid reservoir, third fluid reservoir and the 4th fluid reservoir by pipeline, and the lower end discharge pipe of the ion exchange bed is equipped with multiple In situ ATR-FTIR analyzer;The upper end discharge port of the ion exchange bed is connected with the 4th fluid reservoir by pipeline.The present invention by multiple In situ ATR-FTIR analyzer D1 real-time detection result control valve, avoids the shortcomings that prior art uses cured operation program to practical operation situation difference in response, cannot independently optimize operating parameter convenient for staff.)

1. a kind of low-loss Amine Solutions purification device, including ion exchange bed (X1), it is characterised in that: the ion exchange The upper end feed inlet of bed (X1) has inert gas gas cylinder (C1), the 5th fluid reservoir (T5) and the second fluid filling pump by Pipe installing (P2), it is equipped with first flowmeter (F1) on the outlet pipe of the inert gas gas cylinder (C1), the 5th fluid reservoir (T5) Discharge pipe on the 7th valve (V7) is installed, the lower end feed inlet of the ion exchange bed (X1) is connected with by pipeline The extraction opening of one fluid filling pump (P1), first fluid filling pump (P1) is connected with the first fluid reservoir (T1) by pipeline;

The lower end discharge port of the ion exchange bed (X1) is connected with the second fluid reservoir (T2), third fluid reservoir (T3) by pipeline With the 4th fluid reservoir (T4), the lower end discharge pipe of the ion exchange bed (X1) is equipped with multiple In situ ATR-FTIR analysis Instrument (D1);

The upper end discharge port of the ion exchange bed (X1) is connected with the 4th fluid reservoir (T4), second fluid reservoir by pipeline (T2) it is equipped on feed pipe third valve (V3), the 4th valve is installed on the feed pipe of the third fluid reservoir (T3) Door (V4), the 4th fluid reservoir (T4) connect and are equipped with the 5th valve on the discharge opening pipeline of the lower end ion exchange bed (X1) (V5), the second valve (V2) is installed on the 4th fluid reservoir (T4) the connection upper end ion exchange bed (X1) discharge opening pipeline.

2. a kind of low-loss Amine Solutions purification device according to claim 1, it is characterised in that: second liquid feeding It pumps and is equipped with second flowmeter (F2) on the discharge pipe of (P2), the extraction opening of second fluid filling pump (P2) is connected by pipeline There are third fluid reservoir (T3) and the 6th fluid reservoir (T6).

3. a kind of low-loss Amine Solutions purification device according to claim 2, it is characterised in that: the third liquid storage 6th valve (V6) is installed on the discharge pipe of tank (T3), is equipped with the 8th on the discharge pipe of the 6th fluid reservoir (T6) Valve (V8).

4. a kind of low-loss Amine Solutions purification device according to claim 1, it is characterised in that: first liquid feeding It pumps and third flowmeter (F3) and the first valve (V1) is installed on the discharge pipe of (P1).

5. a kind of low-loss Amine Solutions purification device according to claim 1, it is characterised in that: the fluid reservoir It (T1) is original fluid container, the fluid reservoir (T2) is waste liquid tank, and the fluid reservoir (T3) is circulation alkali flow container, the fluid reservoir (T4) For filtering tank, the fluid reservoir (T5) is deionization water pot.

6. a kind of low-loss Amine Solutions purification device according to claim 2, it is characterised in that: the 6th liquid storage Tank (T6) is net alkali liquid tank.

7. a kind of low-loss Amine Solutions purification device according to claim 1, it is characterised in that: the second fluid reservoir (T2) and at the top of the 4th fluid reservoir (T4) it is equipped with gas discharge outlet.

8. a kind of application method of low-loss Amine Solutions purification device according to any one of claim 1 to 7, It is characterized in that, comprising:

1) purify: Amine Solutions to be clean are contained in the first fluid reservoir (T1), and circulation starts, and open the first fluid filling pump (P1), amine liquid is added by the ion exchange bed bottom (X1), into ion exchange bed in the first valve (V1), the second valve (V2) (X1) solution enters the 4th fluid reservoir (T4) from top after purification, and after purification process runs a period of time, device is replied Original state;

2) inert gas purge: inert gas gas cylinder (C1), first flowmeter (F1) and the 5th valve (V5) are opened, is handed over by ion It changes at the top of bed (X1) and is blown into inert gas, the amine aqueous solution remained in ion exchange bed (X1) is made to be discharged into the 4th fluid reservoir (T4), Device replys original state;

3) it washes: opening the 7th valve (V7), the deionized water in the 5th fluid reservoir (T5) is made to be added to ion exchange from top In bed (X1), the 7th valve (V7) is closed after reaching certain liquid level, deionized water impregnates the exchange of ion exchange bed (X1) intermediate ion Resin for a period of time after, open third valve (V3) and waste liquid be discharged to the second fluid reservoir (T2);

4) inert gas purge: opening inert gas bottle (C1) and first flowmeter (F1), by multiple In situ ATR-FTIR point Analyzer (D1) test result, which manually controls, opens third valve (V3) or the 5th valve (V5), if amine concentration is low in previous step Third valve (V3) is then opened in setting value, is discharged into waste liquid the second fluid reservoir (T2), on the contrary then Open valve V5 arranges waste liquid Enter fluid reservoir T4;;

5) pre- regeneration: manually opened fluid filling pump P2 opens valve V6, valve V3, by the circulation alkali liquor in fluid reservoir T3 from ion Injection at the top of bed X1 is exchanged, eluent ion exchanger resin is regenerated in advance from top to bottom, and the liquid of generation is flowed into fluid reservoir T2 In, device returns to original state;

6) it regenerates: the second fluid filling pump (P2), the 8th valve (V8), the 4th valve (V4) is opened, by alkali in the 6th fluid reservoir (T6) Liquid is injected at the top of the ion exchange bed (X1) by the second fluid filling pump (P2), wash away from top to bottom the impurity of resin surface absorption from Son makes resin regeneration, and waste collection is used as circulation alkali liquor in third fluid reservoir (T3) after elution, and device is restored to initial shape State;

7) inert gas purge: inert gas gas cylinder (C1), first flowmeter F1 and third valve (V3) are opened manually, makes to remain Lye is discharged into the second fluid reservoir (T2) in ion exchange bed (X1), and device returns to original state;

8) circulation is completed, and opens next circulation.

9. application method according to claim 8, which is characterized in that in step 3), such as multiple In situ ATR-FTIR point Amine aqueous solution concentration is higher than setting value in analyzer (D1) monitoring washing waste liquid, then closes third valve (V3), while opening the 5th Valve (V5) flows into highly concentrated waste liquid in the 4th fluid reservoir (T4), and device returns to original state;

The time that gas purges in step 4) is controlled by multiple In situ ATR-FTIR analyzer (D1), if amine in previous step Concentration is higher than setting value and then extends purge time, washing step and inert gas purge step 3) and 4) is then repeated, until outlet Amine concentration is lower than setting value in waste liquid, and system restPoses;

Amine in step 5), in multiple In situ ATR-FTIR analyzer (D1) the record ion exchange bed bottom (X1) outflow waste liquid Concentration reduces in next decontamination cycle multiple Total Reflection Infrared in water-washing step if wherein amine concentration is higher than setting value Spectroanalysis instrument (D1) extends the time of washing and inert gas purge to the decision content of amine concentration;

In step 6), the circulation alkali liquor of multiple In situ ATR-FTIR analyzer (D1) the record ion exchange bed bottom (X1) outflow In amine concentration combine third flowmeter (F3) result to increase stream in subsequent cycle if wherein amine concentration is higher than setting value The amount for entering the amine aqueous solution of ion exchange bed (X1), extends the time of subsequent inert gas purge, and reduces next decontamination cycle Multiple In situ ATR-FTIR analyzer (D1) extends washing and inert blowing gas to the decision content of amine concentration in middle water-washing step The time swept.

Technical field

The invention belongs to solution purifying device technical field, in particular to a kind of low-loss Amine Solutions purification device and Its application method.

Background technique

Petrochemical industry, environmental protection industry (epi) are often used the chemical absorption method based on organic amine absorbent to separate the vulcanization in unstripped gas The sour gas such as hydrogen, carbon dioxide, such as methyl diethanolamine is used in natural gas or synthesis gas from coal gasification depickling gas technique (MDEA) solution removes hydrogen sulfide gas, and monoethanolamine (MEA) removal two is used in power-plant flue gas collecting carbonic anhydride technique Carbon oxide gas.Impurity in unstripped gas participates in reaction or organic amine itself occurs degradation reaction and will lead to Amine Solutions change The problems such as matter, deterioration, effective component constantly reduces in solution, and absorbability constantly declines, even if supplementing organic amine starting materials on time It cannot guarantee that the even running of device, because the product of side reaction caused by impurity and organic amine degradation is mainly with thermal stability The form of salt is accumulated in the solution, and ingredient mainly has formates, acetate, oxalates, sulfate, nitrate, sulfide etc., Thermal stability salinity increases the problems such as will lead to corrosion aggravation, solution foaming, device performance fluctuation.Therefore it need to generally guarantee heat Stable salts concentration is lower than 1.0wt.%.The method for inhibiting thermal-stable salt to generate includes inert gas shielding, is added in solution The methods of additive, but since impurities in feed gas is multifarious, the not high factor of organic amine chemical stability, it is such Method is extremely limited for inhibiting the effect of organic amine deterioration.And thermal stability salt accumulation is let alone, it takes and directly replaces amine liquid Then higher cost, waste liquid are also possible to that environmental problem can be brought method.

How to remove thermal-stable salt is to guarantee one of this kind of desulfurization, the key technology of decarbonization system continuous service, conventional Mechanical filter, activated carbon adsorption purification method not can be removed with thermal-stable salt existing for ionic state.Side used at present Method includes: (1), recuperation of heat method, by the way that alkali is added, so that organic impurities is become high boiling inorganic salts, the method for recycling distillation Low-boiling organic amine component is recycled, but this method energy consumption is higher, the rate of recovery is low, can also introduce higher concentration in systems Alkali;(2), electrodialysis separates foreign ion to the selective penetrated property of different ions using membrane technology, the disadvantage is that separation effect Fruit is bad, film be easy it is contaminated;(3), ion-exchange is comparison used at present a kind of widely method, is handed over using ion Resin is changed to the characteristic of the selective suction-operated of different ions, foreign ion is separated from Amine Solutions, by the way that alkali is added The regeneration for realizing resin adsorption ability, achievees the purpose that resin recycles.

Ion exchange purification device is packed into amberlite in exchange bed container generally centered on ion exchange bed Rouge, purification device are generally run on the branch line of process system, shunted from system a part of solution enter ion exchange bed into Row purification, sets the operation of fixed presetting apparatus, is controlled by control solution flowing velocity in ion exchange bed The time that solution is contacted with resin, after flowing purification continues for some time, by exchanging, the solution discharge in bed is clean, passes through water Wash, alkali liquid regeneration and etc. realize ion exchange resin recycling.Adhesion and suction of this device due to resin to solution Attached effect, device, the problems such as dead volume of pipeline is excessive, feed liquor ratio and residence time is unreasonable can make part solution resident In exchange bed or pipeline, solution system can not be returned to and generate consumption.

Existing purification device control program be it is fixed, can not be made according to solution concentration and purification device operating condition Response.And actually solution concentration is changing always, the absorption property of ion exchange resin also occurs over time Variation, if run only according to fixed parameter, purification system performance just be cannot keep in optimum state, and can occur The problem of excessive solution outlet.

Summary of the invention

The purpose of the present invention is to provide a kind of low-loss Amine Solutions purification device and its application methods, existing to solve Some purification device control programs are fixed, the technology that can not be responded according to solution concentration and purification device operating condition Problem.

To achieve the above object, the invention provides the following technical scheme:

A kind of low-loss Amine Solutions purification device, including ion exchange bed, the upper endfeed of the ion exchange bed Mouth has inert gas gas cylinder, the 5th fluid reservoir and the second fluid filling pump, the escape pipe of the inert gas gas cylinder by Pipe installing First flowmeter is installed on road, the 7th valve, the ion exchange bed are installed on the discharge pipe of the 5th fluid reservoir Lower end feed inlet the first fluid filling pump is connected with by pipeline, the extraction opening of first fluid filling pump is connected with first by pipeline Fluid reservoir;

The lower end discharge port of the ion exchange bed is connected with the second fluid reservoir, third fluid reservoir and the 4th storage by pipeline Flow container, the lower end discharge pipe of the ion exchange bed are equipped with multiple In situ ATR-FTIR analyzer;

The upper end discharge port of the ion exchange bed is connected with the 4th fluid reservoir by pipeline, second fluid reservoir into Third valve is installed on pipe material, the 4th valve, the 4th liquid storage are installed on the feed pipe of the third fluid reservoir The 5th valve is installed on tank connection ion exchange bed lower end discharge opening pipeline, the 4th fluid reservoir connects on ion exchange bed The second valve is installed on the discharge opening pipeline of end.

Further, second flowmeter is installed on the discharge pipe of second fluid filling pump, second fluid filling pump Extraction opening is connected with third fluid reservoir and the 6th fluid reservoir by pipeline.

Further, the 6th valve is installed, the 6th fluid reservoir goes out on the discharge pipe of the third fluid reservoir 8th valve is installed on pipe material.

Further, third flowmeter and the first valve are installed on the discharge pipe of first fluid filling pump.

Further, the fluid reservoir is original fluid container, and the fluid reservoir is waste liquid tank, and the fluid reservoir is circulation alkali liquor Tank, the fluid reservoir are filtering tank, and the fluid reservoir is deionization water pot.

Further, the 6th fluid reservoir is net alkali liquid tank.

Further, gas discharge outlet is equipped at the top of the second fluid reservoir and the 4th fluid reservoir.

A kind of application method of low-loss Amine Solutions purification device, comprising:

1) purify: Amine Solutions to be clean are contained in the first fluid reservoir, and circulation starts, the first fluid filling pump of unlatching, Amine liquid is added by ion exchange bed bottom in first valve, the second valve, into ion exchange bed solution after purification from top Portion enters the 4th fluid reservoir, and after purification process runs a period of time, device replys original state;

2) inert gas purge: opening inert gas gas cylinder, first flowmeter and the 5th valve, by the top of ion exchange bed It is blown into inert gas, makes to remain on the amine aqueous solution in ion exchange bed and is discharged into the 4th fluid reservoir, device replys original state;

3) it washes: opening the 7th valve, be added to the deionized water in the 5th fluid reservoir in ion exchange bed from top, The 7th valve of closing is beaten after deionized water impregnates ion exchange bed ion exchange resin for a period of time after reaching certain liquid level It opens third valve and waste liquid is discharged to the second fluid reservoir;

4) inert gas purge: inert gas bottle and first flowmeter are opened, by multiple In situ ATR-FTIR analyzer Test result, which manually controls, opens third valve or the 5th valve, and the is opened if amine concentration in previous step is lower than setting value Three valves, make waste liquid be discharged into the second fluid reservoir, and on the contrary then Open valve V5 makes waste liquid be discharged into fluid reservoir T4;;

5) pre- regeneration: manually opened fluid filling pump P2 opens valve V6, valve V3, by the circulation alkali liquor in fluid reservoir T3 from Injection at the top of ion exchange bed X1, eluent ion exchanger resin is regenerated in advance from top to bottom, and the liquid of generation is flowed into liquid storage In tank T2, device is returned to original state;

6) it regenerates: opening the second fluid filling pump, the 8th valve, the 4th valve, lye in the 6th fluid reservoir is added by second Liquid pump injects at the top of ion exchange bed, washes away the foreign ion of resin surface absorption from top to bottom, makes resin regeneration, after elution Waste collection is used as circulation alkali liquor into third fluid reservoir, and device returns to original state;

7) inert gas purge: opening inert gas gas cylinder, first flowmeter F1 and third valve manually, make to remain on from Lye is discharged into the second fluid reservoir in son exchange bed, and device returns to original state;

8) circulation is completed, and opens next circulation.

Further, in step 3), such as amine aqueous solution concentration in multiple In situ ATR-FTIR analyzer monitoring washing waste liquid Higher than setting value, then third valve is closed, while opening the 5th valve, flows into highly concentrated waste liquid in the 4th fluid reservoir, device It returns to original state;

The time that gas purges in step 4) is controlled by multiple In situ ATR-FTIR analyzer, if amine in previous step Concentration is higher than setting value and then extends purge time, washing step and inert gas purge step 3) and 4) is then repeated, until outlet Amine concentration is lower than setting value in waste liquid, and system restPoses;

In step 5), the amine in multiple In situ ATR-FTIR analyzer record ion exchange bed bottom outflow waste liquid is dense Degree reduces in next decontamination cycle multiple Total Reflection Infrared light in water-washing step if wherein amine concentration is higher than setting value Spectrum analysis instrument extends the time of washing and inert gas purge to the decision content of amine concentration;

In step 6), in the circulation alkali liquor of multiple In situ ATR-FTIR analyzer record ion exchange bed bottom outflow Amine concentration combines third flowmeter result to increase and flows into ion friendship if wherein amine concentration is higher than setting value in subsequent cycle The amount for changing the amine aqueous solution of bed, extends the time of subsequent inert gas purge, and reduces in next decontamination cycle in water-washing step Multiple In situ ATR-FTIR analyzer extends the time of washing and inert gas purge to the decision content of amine concentration.

Compared with prior art, the beneficial effects of the present invention are: the low-loss Amine Solutions purification device is by multiple Organic amine concentration in solution is discharged in In situ ATR-FTIR analyzer D1 real-time detection ion exchange bed X1, logical convenient for staff The on or off for crossing multiple In situ ATR-FTIR analyzer D1 real-time detection result control valve avoids the prior art using solid The operation program of change is to practical operation situation difference in response, the shortcomings that cannot independently optimizing operating parameter, also, further, this Invention can also measure amine aqueous solution and purification device operation program is combined from the function of main regulation, purification can be filled The amine loss for setting operation key step is information-based, and loss is reduced by optimization operating parameter, reduces operating cost.

Detailed description of the invention

The accompanying drawings constituting a part of this application is used to provide further understanding of the present invention, and of the invention shows Examples and descriptions thereof are used to explain the present invention for meaning property, does not constitute improper limitations of the present invention.In the accompanying drawings:

Fig. 1 is Amine Solutions purification device schematic diagram of the present invention.

In figure: X1 is ion exchange bed, D1 is multiple In situ ATR-FTIR analyzer, C1 is inert gas gas cylinder, F1- It is fluid filling pump, T1-T6 be fluid reservoir, V1-V8 is valve that F3, which is flowmeter, P1 and P2,.

Specific embodiment

The present invention will be described in detail below with reference to the accompanying drawings and embodiments.It should be noted that in the feelings not conflicted Under condition, the features in the embodiments and the embodiments of the present application be can be combined with each other.

Following detailed description is exemplary explanation, it is intended to provide further be described in detail to the present invention.Unless another It indicates, all technical terms of the present invention contain with the normally understood of the application one of ordinary skill in the art Justice is identical.Term used in the present invention is merely to describe specific embodiment, and be not intended to limit according to the present invention Illustrative embodiments.

Referring to Fig. 1, the present invention provides a kind of technical solution: a kind of low-loss Amine Solutions purification device, including from Son exchanges bed X1, and ion exchange bed X1 contains top cover, bottom cover and connected strainer, is packed into amberlite in ion exchange bed X1 Rouge, the ion exchange resin contained in ion exchange bed X1 are that cation exchange resin, anion exchange resin or yin-yang are mixed Ion exchange resin is closed, the strainer for pushing up bottom cover can guarantee that resin will not flow out ion exchange bed X1, and ion exchange bed X1's is upper Endfeed mouth has inert gas gas cylinder C1, fluid reservoir T5 and a fluid filling pump P2 by Pipe installing, in inert gas gas cylinder C1 gas cylinder The gas of splendid attire is the inert gases such as nitrogen, argon gas or helium, is equipped with flowmeter on the outlet pipe of inert gas gas cylinder C1 F1 is equipped with valve V7 on the discharge pipe of fluid reservoir T5, flowmeter F2, fluid filling pump is equipped on the discharge pipe of fluid filling pump P2 The extraction opening of P2 is connected with fluid reservoir T3 and fluid reservoir T6 by pipeline, and valve V6 is equipped on the discharge pipe of fluid reservoir T3, Valve V8 is installed, the lower end feed inlet of ion exchange bed X1 is connected with fluid filling pump by pipeline on the discharge pipe of fluid reservoir T6 The extraction opening of P1, fluid filling pump P1 are connected with fluid reservoir T1 by pipeline, and flowmeter F3 is equipped on the discharge pipe of fluid filling pump P1 Fluid reservoir T2, fluid reservoir T3 and fluid reservoir T4 are connected with by pipeline with the lower end discharge port of valve V1, ion exchange bed X1, from The upper end discharge port of son exchange bed X1 is connected with fluid reservoir T4 by pipeline, and the lower end discharge pipe of ion exchange bed X1 is equipped with The detection window of multiple In situ ATR-FTIR analyzer D1, multiple In situ ATR-FTIR analyzer D1 are embedded into ion exchange The outer wall of bed X1 bottom conduit, window surface are directly contacted with waste liquid, concentration of the measurable flow through organic amine in the liquid of window, Its measurement result divides the duration of each step during decision subsequent purification and number of repetition, multiple In situ ATR-FTIR The material of analyzer D1 infrared spectroscopy window is monocrystalline silicon, zinc selenide, diamond or calcirm-fluoride, is pacified on the feed pipe of fluid reservoir T2 Equipped with valve V3, valve V4, the discharging of the fluid reservoir T4 connection lower end ion exchange bed X1 are installed on the feed pipe of fluid reservoir T3 Valve V5 is installed on mouth pipeline, valve V2 is installed on the discharge opening pipeline of the upper end fluid reservoir T4 connection ion exchange bed X1.

Referring to Fig. 1, fluid reservoir T1 is original fluid container, fluid reservoir T2 is waste liquid tank, and fluid reservoir T3 is circulation alkali flow container, liquid storage Tank T4 is filtering tank, and fluid reservoir T5 is deionization water pot, and fluid reservoir T6 is net alkali liquid tank, is had at the top of fluid reservoir T2, fluid reservoir T4 Gas discharge outlet, being contained in fluid reservoir T6 is the alkali solubles such as sodium hydroxide needed for ion exchange resin regeneration, potassium hydroxide Liquid.

Referring to Fig. 1, device original state is that valve V1-V8, flowmeter F1-F3 are turned off, after device starting under It states step and circuits sequentially operation:

1) purify: Amine Solutions to be clean are contained in fluid reservoir T1, and circulation starts, manually opened fluid filling pump P1, Amine liquid is added by the bottom ion exchange bed X1 in valve V1, valve V2, into ion exchange bed X1 solution after purification from top Portion enters fluid reservoir T4, and after purification process runs a period of time, device replys original state;

2) inert gas purge: inert gas gas cylinder C1, flowmeter F1 and valve V5 are opened manually, by ion exchange bed X1 Top is blown into inert gas, and the amine aqueous solution remained in ion exchange bed X1 is made to be discharged into fluid reservoir T4, and device replys original state;

3) it washes: opening valve V7 manually, the deionized water in fluid reservoir T5 is made to be added to ion exchange bed X1 from top In, valve V7 is closed after reaching certain liquid level, after deionized water impregnates ion exchange bed X1 ion exchange resin for a period of time, Valve V3 is opened manually, and waste liquid is discharged to fluid reservoir T2, such as amine in multiple In situ ATR-FTIR analyzer D1 monitoring washing waste liquid Solution concentration is higher, then it closes valve V3, while Open valve V5, flows into highly concentrated waste liquid in fluid reservoir T4, device is extensive Original state is arrived again;

4) inert gas purge: opening inert gas bottle C1 and flowmeter F1 manually, by multiple In situ ATR-FTIR point Analyzer D1 test result, which manually controls, opens valve V3 or valve V5, opens if amine concentration in previous step is lower than setting value Valve V3, makes waste liquid be discharged into fluid reservoir T2, and on the contrary then Open valve V5 makes waste liquid be discharged into fluid reservoir T4;The time of gas purging It is controlled by multiple In situ ATR-FTIR analyzer D1, when extending purging if amine concentration in previous step is higher than setting value Between, then repeating washing step and inert gas purge step (3) and (4) until amine concentration is lower than setting value in discharging any waste liquor is System restPoses;

5) pre- regeneration: manually opened fluid filling pump P2 opens valve V6, valve V3, by the circulation alkali liquor in fluid reservoir T3 from Injection at the top of ion exchange bed X1, eluent ion exchanger resin is regenerated in advance from top to bottom, and the liquid of generation is flowed into liquid storage In tank T2, device is returned to original state;The bottom the ion exchange bed X1 outflow of multiple In situ ATR-FTIR analyzer D1 record Amine concentration in waste liquid reduces multiple total reflection in water-washing step in next decontamination cycle if wherein amine concentration is higher Infrared spectrometric analyzer D1 extends the time of washing and inert gas purge to the decision content of amine concentration;

6) regenerate: manually opened fluid filling pump P2, valve V8, valve V4, by lye in fluid reservoir T6 by fluid filling pump P2 from Injection at the top of ion exchange bed X1, washes away the foreign ion of resin surface absorption from top to bottom, makes resin regeneration, waste liquid after elution It is collected into fluid reservoir T3 as circulation alkali liquor, device returns to original state;Multiple In situ ATR-FTIR analyzer D1 note Amine concentration in the circulation alkali liquor of the record bottom ion exchange bed X1 outflow is tied in subsequent cycle if wherein amine concentration is higher Collaborate meter F3 result and increase the amount for flowing into the amine aqueous solution of ion exchange bed X1, extends the time of subsequent inert gas purge, and Reduce decision content of the multiple In situ ATR-FTIR analyzer D1 to amine concentration, extension in water-washing step in next decontamination cycle The time of washing and inert gas purge;

7) inert gas purge: opening inert gas gas cylinder C1, flowmeter F1 and valve V3 manually, makes to remain on ion friendship It changes lye in an X1 and is discharged into fluid reservoir T2, device returns to original state;

8) circulation is completed, and opens next circulation.

The low-loss Amine Solutions purification device passes through multiple In situ ATR-FTIR analyzer D1 real-time detection ion Organic amine concentration in bed X1 discharge solution is exchanged, is examined in real time convenient for staff by multiple In situ ATR-FTIR analyzer D1 The on or off for surveying result control valve, avoids the prior art using cured operation program to practical operation situation difference in response, The shortcomings that operating parameter cannot independently be optimized.Also, further, the present invention can also set electrically-controlled valve for valve V1-V7, Multiple In situ ATR-FTIR analyzer D1 detection added input purification device control device, can be corresponded to according to the concentration of detection Automatically control each electrically-controlled valve;The present invention can measure amine aqueous solution and purification device runs program and combines from the function of main regulation To together, informationization is lost in the amine that purification device can be run to key step, and loss, drop are reduced by optimization operating parameter Low operating cost.

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