CN102145256B - Method for separating boron isotopes by simulated moving bed chromatography - Google Patents
Method for separating boron isotopes by simulated moving bed chromatography Download PDFInfo
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Abstract
The invention discloses a method for separating boron isotopes by simulated moving bed chromatography. The method is used to selectively separate isotopes 10B with high thermal-neutron-absorption cross section from boric acid by simulated moving bed chromatograph with a sassolite solution as a raw material, deionized water as a mobile phase, and weak-base anion-exchange resin as a stationary phase. The method comprises the following steps of: preparing a boric acid aqueous solution with certain concentration, filtering the boric acid aqueous solution for removing impurities to obtain a sample injection solution for a simulated moving bed, then loading samples by the simulated moving bed, collecting condensed boric acid rich in isotopes 10B at an extraction port, and then obtaining a target product by evaporation concentration. The method for separating the boron isotopes is continuous and has high separation efficiency.
Description
Technical field
The invention belongs to a kind of isotope separation method, be specifically related to a kind ofly utilize ion-exchange chromatography to combine with simulated moving bed technology to stablize the method for Separation of Boron Isotopes.
Background technology
Boron (B) has two kinds of stable isotopes:
10B and
11B.Wherein
10B has very high thermal neutron absorption cross section (3837 target), is a kind of good reactor control material.Yet, isotope in the natural boron
10The content of B is lower, is 19.78%, and major part is the isotope that thermal neutron absorption cross section only has 0.005 target
11B.Therefore need to two kinds of isotopic separations, obtain richness
10The concentrated boron of B is to improve the neutron-absorbing performance.If the concentrated boric acid of use in reactor cooling system (
10B enriched boric acid, EBA), then can reduce the boric acid concentration in the cooling agent, reduce the radwaste discharge capacity, alleviate the corrosion of zirconium alloy cladding and the stress corrosion cracking of steam generator pipeline, be conducive to nuclear power station and lengthen the life.Yet, because at present the production cost of conversion is too high from sassolite to enrichment boric acid, as for
10The B enrichment is 92% concentrated boron, and the separation costs of chemical exchange method is about 2-3 $/g, and the receptible ceiling price of nuclear power station is 1 $/g.Thereby overslaugh sassolite to enrichment boric acid conversion, therefore in the urgent need to working out a kind of relatively cheap separation method.The patent No. is the method that the United States Patent (USP) " Method ofseparation boron isotopes " of US4447303 discloses a kind of separation by laser boron istope, but the method yields poorly, and is difficult to form large-scale production.
In order to improve the separative efficiency of boron istope, the patent No. is that the United States Patent (USP) of US5443732 discloses a kind of continuous ionic exchange chromatography separation method in " Boron isotope separation using continuous ion exchange chromatography ", it is as raw material take BAS, take weak base type anion exchange resin as exchanger, use the deionized water wash-out, use the annular chromatography Separation of boron isotopes.The method needs ion exchange column to have enough length and width, and therefore certain limitation is arranged when the concentrated boron of the high enrichment of preparation.
In order to improve the enrichment of stablizing boron istope, the patent No. is that the international monopoly of WO2009/138992 A1 has been announced a kind of step ion-exchange chromatography in " An innovative ' cut-and-feed ' operation for enhancing the performance ofion-exchange chromatographic separation ".This inventive method at first forms a light isotope in chromatographic column
10The B abundance zone then will
10The B abundance zone disconnects wash-out, and sassolite adds continuously in the post enrichment and carries out next step wash-out simultaneously.The method can effectively overcome the platform area (42.9%) of abundance zone, and the flow rates of optimization band is 5cm/h～15cm/h, but owing to be non-continued operation, separation cycle increases.
It had both kept the advantage of chromatographic isolation SMBC method (simulated moving bed chromatography, be called for short SMBC), intensive again in the chemical industry continuously, the factors such as adverse current, backflow, make system have the ability that scale separates.In recent years, the SMBC technology is obtaining fast development aspect the medicine separation, still, still has no so far open report for the method for using the SMBC Separation of boron isotopes.
Summary of the invention
The object of the present invention is to provide a kind of have high separative efficiency and the low method of utilizing the SMBC Separation of boron isotopes of production cost.
Technical scheme of the present invention is as follows:
Utilize the method for SMBC Separation of boron isotopes, it is characterized in that: described method concrete steps are as follows:
Step 1: preparation boric acid aqueous solution
The boric acid solid is placed beaker, add distilled water, stirring and dissolving; In solution injection capacity bottle, wash beaker with distillation, and washing lotion is poured in the volumetric flask, be mixed with boric acid aqueous solution;
Step 2: filtering and impurity removing
With the BAS membrane filtration, remove the impurity in the solution, ultrasonic degas obtains simulation moving-bed sample introduction liquid;
Step 3: evaporation and concentration
Sample introduction liquid is added in the separation system of simulated moving bed chromatography continuously, use simultaneously the deionized water wash-out, set simulation moving-bed subregion flow velocity and port switching time and running temperature; After simulated moving bed system reaches poised state, collect enriched isotope in simulation moving-bed extract port
10The concentrated BAS of B places drying oven to carry out inspissation the BAS of collecting, the solid boric acid that obtains concentrating.
Simulation moving-bed chromatographic column in the described step 3 is divided into I～IV district; Wherein prop up chromatographic column by 2-6 and form in the II district, and each is comprised of I district and III district 2 chromatographic columns, and the IV district is comprised of 0～2 chromatographic column; I district flow velocity is 51cm/h～85cm/h; II district flow velocity is 45cm/h～76cm/h; III district flow velocity is 46cm/h～84cm/h; IV district flow velocity is 0cm/h～5cm/h; Port switching time is 15min～30min; Running temperature is 10 ℃～40 ℃.
Filler in the described SMBC post is weak-base anion-exchange resin.
Described weak-base anion-exchange resin is D301-G or DIAN resin.
The concentration of the described step 1 mesoboric acid aqueous solution is 6g/L-30g/L boric acid.
The ultrasonic degas time in the described step 2 is 10min～15min.
The temperature of described step 3 mesoboric acid solution inspissation in drying oven is 50 ℃-90 ℃.
Effect of the present invention is: compare with the Separation of Boron Isotopes method of background technology, Separation of Boron Isotopes method of the present invention is a kind of method of continuous Separation of boron isotopes, and separative efficiency is high; Compare chemical exchange method, the method can effectively reduce the production cost of concentrated boron.
The specific embodiment
Method of the present invention is take sassolite solution as raw material, take deionized water as mobile phase, take weak-base anion-exchange resin as fixing phase, optionally isolates the isotope with high thermal neutron absorption cross section with SMBC from boric acid
10B.By preparing certain density boric acid aqueous solution, with the BAS filtering and impurity removing, obtain simulation moving-bed sample introduction liquid, then simulation moving-bed loading is collected enriched isotope in extract port
10The concentrated boric acid of B, evaporation and concentration obtains target product.
The simulation moving-bed be comprised of 8～12 chromatographic columns that the weak-base anion-exchange resin filler of particle mean size 0.28mm is housed of the present invention's employing, weak-base anion-exchange resin is D301-G or DIAN resin.The ratio of height to diameter of chromatographic column 10: 1; Chromatographic column is divided into I～IV district; Wherein prop up chromatographic column by 2-6 and form in the II district, and each is comprised of I district and III district 2 chromatographic columns, and the IV district is comprised of 0～2 chromatographic column; I district flow velocity is 51cm/h～85cm/h; II district flow velocity is 45cm/h～76cm/h; III district flow velocity is 46cm/h～84cm/h; IV district flow velocity is 0cm/h～5cm/h; Port switching time is 15min～30min; Running temperature is 10 ℃～40 ℃.
Concrete steps are as follows:
Step 1: preparation boric acid aqueous solution
The boric acid solid is placed beaker, add distilled water, stirring and dissolving; In solution injection capacity bottle, to wash beaker with distillation, and washing lotion is poured in the volumetric flask, last constant volume shakes all, is mixed with boric acid aqueous solution;
Step 2: filtering and impurity removing
With the BAS membrane filtration, remove the impurity in the solution, then carry out ultrasonic degas, obtain simulation moving-bed sample introduction liquid;
Step 3: evaporation and concentration
Sample introduction liquid is added in the separation system of simulated moving bed chromatography continuously, use simultaneously the deionized water wash-out, set simulation moving-bed subregion flow velocity and port switching time; After simulated moving bed system reaches poised state, collect enriched isotope in simulation moving-bed extract port
10The concentrated BAS of B places drying oven with the BAS of collecting, and in 50 ℃ of-90 ℃ of temperature ranges, carries out inspissation, obtains thickened solid boric acid.
Below, in conjunction with the embodiments method of the present invention is further described:
Embodiment 1
Step 1: preparation boric acid aqueous solution
Get boric acid solid 3g with electronic balance scale and place beaker, add distilled water, stirring and dissolving; Solution is injected the 500ml volumetric flask, wash beaker 3 times with distillation, washing lotion is poured in the volumetric flask, constant volume shakes all, is made into the BAS of 6g/L;
Step 2: filtering and impurity removing
BAS with 0.45 μ m membrane filtration, is removed the impurity in the solution, then the boric acid aqueous solution behind the suction filtration is carried out ultrasonic degas, ultrasonic degas time 10min obtains simulation moving-bed sample introduction liquid.Simulation moving-bedly formed the ratio of height to diameter of chromatographic column 10: 1 by 8 chromatographic columns; 8 chromatographic columns are divided into 4 districts, and every district is comprised of 2 chromatographic columns; Chromatographic column filler is that particle mean size is the DIAN weak-base anion-exchange resin of 0.28mm, 30 ℃ of simulation moving-bed running temperatures.
Step 3: evaporation and concentration
Sample introduction liquid is added in the separation system of simulated moving bed chromatography continuously, use simultaneously the deionized water wash-out, setting I district flow velocity is 85cm/h, and II district flow velocity is 76cm/h; III district flow velocity is 84cm/h; IV district flow velocity is 10cm/h; Port switching time is 15min; After simulated moving bed system reaches poised state, collect rich in simulation moving-bed extract port
10The BAS of B places drying oven with the BAS of collecting, and carries out inspissation under 50 ℃ of temperature, obtains
10The B enrichment is 25% solid boric acid.
Embodiment 2
Step 1: preparation boric acid aqueous solution
Get boric acid solid 15g with electronic balance scale and place beaker, add distilled water, stirring and dissolving; Solution is injected the 500ml volumetric flask, wash beaker 3 times with distillation, washing lotion is poured in the volumetric flask, constant volume shakes all, is made into the BAS of 30g/L;
Step 2: filtering and impurity removing
BAS with 0.45 μ m membrane filtration, is removed the impurity in the solution, then the boric acid aqueous solution behind the suction filtration is carried out ultrasonic degas, ultrasonic degas time 12min obtains simulation moving-bed sample introduction liquid.Simulation moving-bedly formed by 8 chromatographic columns, the ratio of height to diameter of chromatographic column 10: 1,8 chromatographic columns are divided into 3 districts, and wherein the II district is comprised of 4 chromatographic columns, and I district and III district are comprised of 2 chromatographic columns; Chromatographic column filler is that particle mean size is the DIAN weak-base anion-exchange resin of 0.28mm; 10 ℃ of simulation moving-bed running temperatures.
Step 3: evaporation and concentration
Sample introduction liquid is added in the separation system of simulated moving bed chromatography continuously, use simultaneously the deionized water wash-out, setting I district flow velocity is 68cm/h, and II district flow velocity is 61cm/h; III district flow velocity is 63cm/h; Port switching time is 20min; After simulated moving bed system reaches poised state, collect BAS in extract port, the BAS of collecting is placed drying oven, under 70 ℃ of temperature, carry out inspissation, obtain
10The B enrichment is 45% solid boric acid.
Embodiment 3
Step 1: preparation boric acid aqueous solution
Get boric acid solid 6g with electronic balance scale and place beaker, add distilled water, stirring and dissolving; Solution is injected the 500ml volumetric flask, wash beaker 2 times with distillation, washing lotion is poured in the volumetric flask, constant volume shakes all, is made into the BAS of 12g/L;
Step 2: filtering and impurity removing
BAS with 0.45 μ m membrane filtration, is removed the impurity in the solution, then the boric acid aqueous solution behind the suction filtration is carried out ultrasonic degas, ultrasonic degas time 15min obtains simulation moving-bed sample introduction liquid.Simulation moving-bedly be comprised of 12 chromatographic columns, be divided into 4 districts, wherein the II district is comprised of 6 chromatographic columns, and each is comprised of I district, III district, IV district 2 chromatographic columns; Chromatographic column filler is that particle mean size is the D301-G weak-base anion-exchange resin of 0.28mm; 40 ℃ of simulation moving-bed running temperatures.
Step 3: evaporation and concentration
Sample introduction liquid is added in the separation system of simulated moving bed chromatography continuously, use simultaneously the deionized water wash-out, setting I district flow velocity is 51cm/h, and II district flow velocity is 45cm/h; III district flow velocity is 46cm/h; IV district flow velocity is 5cm/h; Port switching time is 30min; After simulated moving bed system reaches poised state, collect BAS in extract port, the BAS of collecting is placed drying oven, under 90 ℃ of temperature, carry out inspissation, obtain through inspissation
10The B enrichment is 80% solid boric acid.
Select the chromatographic column filler (particle mean size be the DIAN weak-base anion-exchange resin of 0.28mm) identical with embodiment 1, identical raw material (concentration is the BAS of 6g/L), and identical running temperature (30 ℃) and chromatographic column specification, carry out the experiment of simulated moving bed chromatographic separation process and batch (-type) ion-exchange chromatography separation method Separation of boron isotopes, the separating property of two kinds of separation methods such as following table:
SMBC and batch (-type) ion-exchange chromatography Separation of boron isotopes separating effect are relatively
As can be seen from the above table, produce same enrichment and be 25% concentrated boric acid, separate with SMBC, the output between unit is about 4.7 times of batch (-type) ion-exchange chromatography output.
Claims (2)
1. utilize the method for SMBC Separation of boron isotopes, concrete steps are as follows:
Step 1: preparation boric acid aqueous solution
The boric acid solid is placed beaker, add distilled water, stirring and dissolving; In solution injection capacity bottle, wash beaker with distillation, and washing lotion is poured in the volumetric flask, be mixed with the boric acid aqueous solution that concentration is 6g/L-30g/L;
Step 2: filtering and impurity removing
With the BAS membrane filtration that makes, remove the impurity in the solution, use again ultrasonic degas 10-15min, obtain simulation moving-bed sample introduction liquid;
Step 3: evaporation and concentration
In separation system of simulated moving bed chromatography, be set to I～IV district with simulation moving-bed; Wherein prop up chromatographic column by 2-6 and form in the II district, and each is comprised of I district and III district 2 chromatographic columns, and the IV district is comprised of 0～2 chromatographic column; Filler is weak-base anion-exchange resin in the chromatographic column; Setting simulation moving-bed I district flow velocity is 51cm/h～85cm/h; II district flow velocity is 45cm/h～76cm/h; III district flow velocity is 46cm/h～84cm/h; IV district flow velocity is 0cm/h～5cm/h; Setting port switching time is 15min～30min; Running temperature is 10 ℃～40 ℃;
Sample introduction liquid is added in the separation system of simulated moving bed chromatography continuously, use simultaneously the deionized water wash-out, after simulated moving bed system reaches poised state, collect enriched isotope in simulation moving-bed extract port
10The concentrated BAS of B; With what collect
10The B BAS places drying oven to carry out inspissation, the solid that obtains concentrating under 50 ℃ of-90 ℃ of temperature
10B boric acid.
2. according to the method for utilizing the SMBC Separation of boron isotopes claimed in claim 1, it is characterized in that: the filler in the described chromatographic column--weak-base anion-exchange resin is D301-G or DIAN resin.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103623700A (en) * | 2013-10-30 | 2014-03-12 | 天津大学 | Method for separating boron isotopes by taking boron-specific resin as simulated moving bed stationary phase |
| CN104226112A (en) * | 2014-09-26 | 2014-12-24 | 中国科学院青海盐湖研究所 | Boron isotope separation method |
| CN104729906B (en) * | 2015-04-14 | 2017-05-03 | 中国科学院地球环境研究所 | Efficient and pollution-free boron isotope pressurization separating device for low-boron environmental samples |
| CN107096383A (en) * | 2017-05-04 | 2017-08-29 | 天津大学 | The purposes of metal-organic framework materials Separation of boron isotopes |
| CN107020014A (en) * | 2017-05-04 | 2017-08-08 | 天津大学 | Using metal-organic framework materials as the method for Simulation moving bed stationary phase Separation of boron isotopes |
| CN107008150A (en) * | 2017-05-04 | 2017-08-04 | 天津大学 | Using catechol chelating resin as the method for Simulation moving bed stationary phase Separation of boron isotopes |
| CN107261846B (en) * | 2017-06-21 | 2021-03-09 | 中国科学院过程工程研究所 | Method for continuously separating enriched boron isotopes by ion exchange chromatography based on gradient elution |
| CN107413195A (en) * | 2017-08-21 | 2017-12-01 | 天津大学 | In the method that MOF 74 (Zn) is Simulation moving bed stationary phase Separation of boron isotopes |
| CN107376646A (en) * | 2017-08-21 | 2017-11-24 | 天津大学 | Method using metal-organic framework materials as Simulation moving bed stationary phase Separation of boron isotopes |
| CN110143600A (en) * | 2019-05-27 | 2019-08-20 | 天津纯态化学工程技术有限公司 | A kind of method of the separating-purifying of boron -10 and boron -11 |
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| JPS60102946A (en) * | 1983-11-11 | 1985-06-07 | Mitsubishi Chem Ind Ltd | Anion exchange resin for separating boron isotope |
| JPH0221925A (en) * | 1988-07-11 | 1990-01-24 | Sumitomo Heavy Ind Ltd | Method for concentrating boron isotope by moving bed |
| US5443732A (en) * | 1994-04-01 | 1995-08-22 | Westinghouse Electric Corporation | Boron isotope separation using continuous ion exchange chromatography |
| CN1169595C (en) * | 2002-03-13 | 2004-10-06 | 浙江大学 | Analogue mobile bed chromatic reactor |
| JP2008029989A (en) * | 2006-07-31 | 2008-02-14 | Sumitomo Metal Mining Co Ltd | Method for separating and recovering boron form boron-containing water |
| CN100551497C (en) * | 2007-12-26 | 2009-10-21 | 中国核动力研究设计院 | Technology with boron resin ion-exchange chromatography Separation of boron isotopes |
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