CN110420480B - Method for removing ammonium alkylbenzenesulfonate from carbonate precipitant for rare earth - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 35
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 title claims abstract description 33
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 title claims abstract description 18
- 229910052761 rare earth metal Inorganic materials 0.000 title claims description 52
- 150000002910 rare earth metals Chemical class 0.000 title claims description 34
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical group [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 55
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 55
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims abstract description 51
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 51
- 239000007864 aqueous solution Substances 0.000 claims abstract description 36
- 239000011347 resin Substances 0.000 claims abstract description 35
- 229920005989 resin Polymers 0.000 claims abstract description 35
- CHRJZRDFSQHIFI-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;styrene Chemical compound C=CC1=CC=CC=C1.C=CC1=CC=CC=C1C=C CHRJZRDFSQHIFI-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229920001577 copolymer Polymers 0.000 claims abstract description 31
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 8
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- 230000001376 precipitating effect Effects 0.000 claims abstract description 8
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 6
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 5
- 235000012501 ammonium carbonate Nutrition 0.000 claims abstract description 4
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims abstract description 4
- 235000017557 sodium bicarbonate Nutrition 0.000 claims abstract description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 4
- 235000017550 sodium carbonate Nutrition 0.000 claims abstract description 4
- 239000002253 acid Substances 0.000 claims abstract 2
- -1 ammonium alkyl benzene Chemical class 0.000 claims description 50
- 229940077388 benzenesulfonate Drugs 0.000 claims description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000002245 particle Substances 0.000 claims description 10
- 150000004996 alkyl benzenes Chemical class 0.000 claims description 8
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 8
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 5
- 125000005210 alkyl ammonium group Chemical group 0.000 claims 1
- 239000012535 impurity Substances 0.000 abstract description 13
- 239000000243 solution Substances 0.000 description 24
- PLUHAVSIMCXBEX-UHFFFAOYSA-N azane;dodecyl benzenesulfonate Chemical compound N.CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 PLUHAVSIMCXBEX-UHFFFAOYSA-N 0.000 description 9
- 238000001914 filtration Methods 0.000 description 8
- 239000012716 precipitator Substances 0.000 description 8
- 238000001179 sorption measurement Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000007787 solid Substances 0.000 description 7
- 229920000642 polymer Polymers 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 238000010557 suspension polymerization reaction Methods 0.000 description 2
- MGSRCZKZVOBKFT-UHFFFAOYSA-N thymol Chemical compound CC(C)C1=CC=C(C)C=C1O MGSRCZKZVOBKFT-UHFFFAOYSA-N 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000005844 Thymol Substances 0.000 description 1
- 125000004390 alkyl sulfonyl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- 239000002241 glass-ceramic Substances 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229960000790 thymol Drugs 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
- B01J20/267—Cross-linked polymers
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
本发明公开了一种从稀土用碳酸盐类沉淀剂中脱除烷基苯磺酸铵的方法，包括如下步骤：形成含稀土用碳酸盐类沉淀剂的水溶液，所述水溶液含有烷基苯磺酸铵；将所述水溶液以30～80L/h的流量通过苯乙烯‑二乙烯基苯交联共聚物填充的树脂柱，从而除去所述水溶液中的烷基苯磺酸铵；其中，稀土用碳酸盐类沉淀剂为碳酸氢铵、碳酸铵、碳酸钠或碳酸氢钠；所述烷基苯磺酸铵的烷基含有5～25个碳原子。该方法可以有效除去烷基苯磺酸铵杂质。The invention discloses a method for removing ammonium alkylbenzenesulfonate from a carbonate precipitant for rare earths. The method includes the following steps: forming an aqueous solution containing a carbonate precipitant for rare earths, the aqueous solution containing alkylbenzenesulfonate Ammonium acid; passing the aqueous solution through a resin column filled with styrene-divinylbenzene cross-linked copolymer at a flow rate of 30-80 L/h, thereby removing the ammonium alkylbenzenesulfonate in the aqueous solution; The carbonate precipitating agent is ammonium bicarbonate, ammonium carbonate, sodium carbonate or sodium bicarbonate; the alkyl group of the ammonium alkylbenzenesulfonate contains 5-25 carbon atoms. The method can effectively remove ammonium alkylbenzenesulfonate impurities.
Description
Technical Field
The invention relates to a method for removing ammonium alkyl benzene sulfonate from a precipitant for rare earth, in particular to a method for removing ammonium alkyl benzene sulfonate from a carbonate precipitant for rare earth.
Background
Rare earth elements are known as industrial vitamins, have irreplaceable excellent magnetic, optical and electrical properties, and play a great role in improving product performance, increasing product varieties and improving production efficiency. Because of large action and small dosage of rare earth, the rare earth has become an important element for improving the product structure, improving the technological content and promoting the technical progress of the industry, and is widely applied to the fields of metallurgy, military, petrochemical industry, glass ceramics, agriculture, new materials and the like.
The rare earth carbonate is an intermediate raw material for preparing various rare earth products, has wide application and plays an extremely important role. The rare earth carbonate can be prepared by adding a precipitator into single or mixed rare earth chloride feed liquid, rare earth sulfate feed liquid or rare earth nitrate feed liquid obtained by extraction and separation. To prevent the precipitant from caking, it is common to add to the precipitant an amount of surfactant, for example: alkyl sulfonyl chlorides, ammonium alkyl benzene sulfonates, and the like. When the rare earth carbonate product is prepared, the surfactant added into the precipitator is adsorbed to the surface of the rare earth carbonate crystal grains, so that the oil content in the rare earth carbonate crystal grains is increased, the washing removal of impurities carried by the rare earth carbonate is hindered, and the surfactant can also increase the content of other impurities, so that the purity of the prepared rare earth carbonate is not high.
Chinese patent application No. 201010241210.1 discloses a method of filtering a precipitant to remove oil by placing the precipitant in a filter tank containing an adsorbent. The adsorbent is one of active carbon, plant ash or rice husk ash. Chinese patent application No. 201711027536.2 discloses a method of removing oil from a precipitant by passing it through a fiber ball. Chinese patent application No. 201010521690.7 discloses a method for preparing oil-free rare earth carbonate by flowing ammonium bicarbonate solution through a head tank into a chemical fiber filter column to remove oil contained in ammonium bicarbonate. Chinese patent application No. 201811342456.0 discloses an impurity and oil removing device for ammonium bicarbonate solution, in which a fiber ball filter is also used to remove oil from the ammonium bicarbonate solution. The above methods can only remove oil which is not easy to dissolve in water, but ammonium alkyl benzene sulfonate which is easy to dissolve in water can not be completely removed by the above methods, so that the content of ammonium alkyl benzene sulfonate impurities in the precipitating agent can not be effectively reduced.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a method for removing ammonium alkylbenzene sulfonate from a carbonate precipitant for rare earth, which is convenient to operate and can effectively remove ammonium alkylbenzene sulfonate impurities. The invention further aims to provide a method for removing ammonium alkyl benzene sulfonate from a carbonate precipitator for rare earth, wherein an adsorption material can be recycled, and industrial production is facilitated.
The invention provides a method for removing ammonium alkyl benzene sulfonate from a carbonate precipitator for rare earth, which comprises the following steps: forming an aqueous solution containing a carbonate precipitant for the rare earth, the aqueous solution containing ammonium alkyl benzene sulfonate; enabling the aqueous solution to pass through a resin column filled with a styrene-divinylbenzene crosslinked copolymer at a flow rate of 30-80L/h, so as to remove ammonium alkyl benzene sulfonate in the aqueous solution;
wherein, the carbonate precipitant for rare earth is ammonium bicarbonate, ammonium carbonate, sodium carbonate or sodium bicarbonate; the alkyl group of the ammonium alkyl benzene sulfonate contains 5-25 carbon atoms.
According to the method, the concentration of the carbonate precipitating agent for the rare earth in the aqueous solution is preferably 1-6 mol/L.
According to the method, preferably, the ammonium alkyl benzene sulfonate in the aqueous solution accounts for 0.005-0.05 wt% of the weight of the carbonate precipitating agent for the rare earth.
According to the method, preferably, the ammonium alkyl benzene sulfonate in the aqueous solution accounts for 0.005-0.03 wt% of the weight of the carbonate precipitating agent for the rare earth.
According to the method of the present invention, preferably, the styrene-divinylbenzene crosslinked copolymer has a specific surface area of not less than 900m2(ii)/g, and the phenol absorption amount is 70mg/ml or more.
According to the method of the present invention, preferably, the styrene-divinylbenzene crosslinked copolymer has a wet apparent density of 0.50 to 0.90g/ml and a wet true density of 1.00 to 1.50 g/ml.
According to the method of the present invention, it is preferable that the styrene-divinylbenzene crosslinked copolymer is a resin particle having a particle diameter ranging from 0.2mm to 2.00mm containing 85% to 100%.
According to the method of the present invention, the ratio of the diameter to the height of the resin column is preferably 1:5 to 17.
According to the preparation method of the invention, the flow rate of the aqueous solution is preferably 30-50L/h.
According to the preparation method of the invention, the flow rate of the aqueous solution is preferably 30-40L/h.
The method adopts the styrene-divinylbenzene cross-linked copolymer to remove the ammonium alkyl benzene sulfonate in the carbonate precipitator for the rare earth, can effectively reduce the content of the ammonium alkyl benzene sulfonate in the carbonate precipitator for the rare earth, and has convenient operation and good removal effect. The resin is used as the adsorption material, so that the regeneration and the reutilization of the adsorption material are conveniently realized, and the industrial production is facilitated. In a preferred embodiment of the present invention, the styrene-divinylbenzene crosslinked copolymer has a specific surface area of not less than 900m2The phenol absorption amount is more than or equal to 70mg/ml, the adsorption capacity of the crosslinked styrene-divinylbenzene polymer can be ensured, and the removal effect of ammonium alkyl benzene sulfonate in the carbonate precipitator for rare earth is enhanced.
Detailed Description
The present invention will be further described with reference to the following specific examples, but the scope of the present invention is not limited thereto.
The carbonate precipitant for rare earth is used for preparing rare earth carbonate. The method for removing ammonium alkyl benzene sulfonate from the carbonate precipitant for rare earth comprises the following steps: forming an aqueous solution containing a carbonate precipitant for the rare earth, the aqueous solution containing ammonium alkyl benzene sulfonate; passing the aqueous solution through a resin column packed with a styrene-divinylbenzene crosslinked copolymer to remove ammonium alkylbenzene sulfonate from the aqueous solution.
In the invention, the carbonate precipitant for rare earth is selected from one or more of ammonium bicarbonate, ammonium carbonate, sodium carbonate or sodium bicarbonate. According to one embodiment of the present invention, the carbonate-based precipitant for rare earth is ammonium bicarbonate.
In the present invention, the alkyl group of ammonium alkylbenzene sulfonate contains 5 to 25 carbon atoms. In certain embodiments, the alkyl group of the ammonium alkyl benzene sulfonate contains 10 to 15 carbon atoms; preferably 10 to 12 carbon atoms. According to one embodiment of the present invention, the ammonium alkylbenzene sulfonate may be ammonium dodecylbenzene sulfonate.
In the invention, the concentration of the carbonate precipitant for rare earth in the aqueous solution is 1-6 mol/L. In some embodiments, the concentration of the carbonate precipitant for the rare earth in the aqueous solution is 2-5 mol/L; preferably 2.5 to 3.5 mol/L. Thus, the effect of removing ammonium alkyl benzene sulfonate in the carbonate precipitant for rare earth can be ensured.
In the invention, ammonium alkyl benzene sulfonate in the aqueous solution accounts for 0.005-0.05 wt% of the weight of the carbonate precipitant for the rare earth. In certain embodiments, the ammonium alkylbenzene sulfonate in the aqueous solution is 0.005 to 0.03 weight percent of the carbonate based precipitant for the rare earth; preferably 0.005 to 0.01 wt%. This can improve the effect of removing ammonium alkyl benzene sulfonate.
In the present invention, the styrene-divinylbenzene crosslinked copolymer can be obtained by a conventional method. For example, styrene and divinylbenzene are subjected to suspension polymerization to obtain a crosslinked styrene-divinylbenzene polymer. The crosslinked styrene-divinylbenzene polymer of the present invention is not limited to one obtained by suspension polymerization, but may be obtained by a conventional method such as solution polymerization, emulsion polymerization, and the like.
In the present invention, the styrene-divinylbenzene crosslinked copolymer has a specific surface area of not less than 900m2(ii)/g, and the phenol absorption amount is 70mg/ml or more. In certain embodiments, the styrene-divinylbenzene crosslinked copolymer has a specific surface area of not less than 1000m2A/g, preferably not less than 1200m2(ii) in terms of/g. In certain embodiments, the styrene-divinylbenzene crosslinked copolymer has a phenolic absorption of 80mg/ml or greater; preferably greater than or equal to 90 mg/ml. Thus, the adsorption capacity of the polymer can be ensured, and a better removal effect can be achieved.
In the present invention, the styrene-divinylbenzene crosslinked copolymer has a wet apparent density of 0.50 to 0.90g/ml and a wet true density of 1.00 to 1.50 g/ml. In certain embodiments, the styrene-divinylbenzene crosslinked copolymer has a wet apparent density of 0.60 to 0.80g/ml, preferably 0.65 to 0.75 g/ml. In certain embodiments, the styrene-divinylbenzene crosslinked copolymer has a wet bulk density of 1.00 to 1.30g/ml, preferably 1.05 to 1.15 g/ml. Thus, the adsorption capacity of the polymer can be ensured, and a better removal effect can be achieved.
In the present invention, the styrene-divinylbenzene crosslinked copolymer is a resin particle containing 85 to 100% of particles having a diameter in the range of 0.2 to 2.00 mm. In certain embodiments, the styrene-divinylbenzene crosslinked copolymer is a resin particle having a particle diameter ranging from 0.4 to 1.25mm containing 90 to 100%. Preferably, the styrene-divinylbenzene crosslinked copolymer is a resin particle having a particle diameter of 0.4 to 1.25mm in a range of 95 to 100%. The granular resin has more uniform pore size, is beneficial to desorbing the adsorbed organic matters in the granular resin so as to complete the regeneration and the reutilization of the resin, and can ensure the effect of removing the ammonium alkyl benzene sulfonate in the carbonate precipitator for the rare earth.
In the invention, the ratio of the diameter to the height of the resin column is 1: 5-17. In some embodiments, the resin column has a diameter to height ratio of 1:6 to 15; preferably, the ratio of the diameter to the height of the resin column is 1:7 to 12. According to one embodiment of the invention, the ratio of the diameter to the height of the resin column is 1: 10. Thus, the adsorption rate can be ensured, and the resin can be fully utilized to reach the maximum adsorption capacity.
In the invention, rare earth is treated by a resin column filled with a styrene-divinylbenzene crosslinked copolymer by using a carbonate precipitant aqueous solution according to the flow rate of 30-80L/h. In some embodiments, the flow rate of the carbonate precipitant aqueous solution for rare earth is 30 to 50L/h. According to one embodiment of the invention, the flow rate of the carbonate precipitant aqueous solution for rare earth is 30-40L/h. Therefore, the ammonium alkyl benzene sulfonate in the aqueous solution can be fully adsorbed and diffused, and the removal efficiency of the ammonium alkyl benzene sulfonate in the aqueous solution can be ensured.
See the following table for the properties of the styrene-divinylbenzene crosslinked copolymers used in the examples below.
TABLE 1
The ammonium alkylbenzene sulfonate content in the aqueous solutions of carbonate-based precipitants for rare earth in the following examples was measured by the following method:
two-phase titration method: the content of ammonium dodecylbenzenesulfonate was determined by two-phase titration using a mixture of thymol blue-methylene blue as an indicator and methylene chloride as a solvent.
Example 1
Solid ammonium bicarbonate (ammonium dodecylbenzene sulfonate accounts for 0.01 wt% of the weight of the ammonium bicarbonate) is dissolved in water, impurities which are not dissolved in the water are removed by filtration, and an ammonium bicarbonate solution with the ammonium bicarbonate concentration of 2.5mol/L is obtained. The ammonium bicarbonate solution was passed through a styrene-divinylbenzene crosslinked copolymer-filled resin column at room temperature. The flow rate was 50L/h, and the diameter of the resin column was 0.3 m and the height was 3 m. The properties of the ammonium bicarbonate solution after removal of the ammonium alkyl benzene sulfonate are shown in table 2.
Example 2
Solid ammonium bicarbonate (ammonium dodecylbenzene sulfonate is 0.005 wt% of the weight of the ammonium bicarbonate) is dissolved in water, impurities which are not dissolved in the water are removed by filtration, and an ammonium bicarbonate solution with the ammonium bicarbonate concentration of 3mol/L is obtained. The ammonium bicarbonate solution was passed through a styrene-divinylbenzene crosslinked copolymer-filled resin column at room temperature. The flow rate was 50L/h, and the diameter of the resin column was 0.3 m and the height was 3 m. The properties of the ammonium bicarbonate solution after removal of the ammonium alkyl benzene sulfonate are shown in table 2.
Example 3
Solid ammonium bicarbonate (ammonium dodecylbenzene sulfonate accounts for 0.03 wt% of the weight of the ammonium bicarbonate) is dissolved in water, impurities which are not dissolved in the water are removed by filtration, and an ammonium bicarbonate solution with the ammonium bicarbonate concentration of 3.5mol/L is obtained. The ammonium bicarbonate solution was passed through a styrene-divinylbenzene crosslinked copolymer-filled resin column at room temperature. The flow rate was 50L/h, and the diameter of the resin column was 0.3 m and the height was 3 m. The properties of the ammonium bicarbonate solution after removal of the ammonium alkyl benzene sulfonate are shown in table 2.
Example 4
Solid ammonium bicarbonate (ammonium dodecylbenzene sulfonate is 0.02 wt% of the weight of the ammonium bicarbonate) is dissolved in water, impurities which are not dissolved in the water are removed by filtration, and an ammonium bicarbonate solution with the ammonium bicarbonate concentration of 3.5mol/L is obtained. The ammonium bicarbonate solution was passed through a styrene-divinylbenzene crosslinked copolymer-filled resin column at room temperature. The flow rate was 30L/h, and the diameter of the resin column was 0.3 m and the height was 3 m. The properties of the ammonium bicarbonate solution after removal of the ammonium alkyl benzene sulfonate are shown in table 2.
Example 5
Solid ammonium bicarbonate (ammonium dodecylbenzene sulfonate accounts for 0.03 wt% of the weight of the ammonium bicarbonate) is dissolved in water, impurities which are not dissolved in the water are removed by filtration, and an ammonium bicarbonate solution with the ammonium bicarbonate concentration of 3.5mol/L is obtained. The ammonium bicarbonate solution was passed through a styrene-divinylbenzene crosslinked copolymer-filled resin column at room temperature. The flow rate was 70L/h, and the diameter of the resin column was 0.3 m and the height was 3 m. The properties of the ammonium bicarbonate solution after removal of the ammonium alkyl benzene sulfonate are shown in table 2.
Comparative example 1
Solid ammonium bicarbonate (ammonium dodecylbenzene sulfonate accounts for 0.03 wt% of the weight of the ammonium bicarbonate) is dissolved in water, impurities which are not dissolved in the water are removed by filtration, and an ammonium bicarbonate solution with the ammonium bicarbonate concentration of 3mol/L is obtained. The ammonium bicarbonate solution was passed through a styrene-divinylbenzene crosslinked copolymer-filled resin column at room temperature. The flow rate was 90L/h, and the diameter of the resin column was 0.3 m and the height was 3 m. The properties of the ammonium bicarbonate solution after removal of the ammonium alkyl benzene sulfonate are shown in table 2.
Comparative example 2
Solid ammonium bicarbonate (ammonium dodecylbenzene sulfonate accounts for 0.07 wt% of the weight of the ammonium bicarbonate) is dissolved in water, impurities which are not dissolved in the water are removed by filtration, and an ammonium bicarbonate solution with the ammonium bicarbonate concentration of 3mol/L is obtained. The ammonium bicarbonate solution was passed through a styrene-divinylbenzene crosslinked copolymer-filled resin column at room temperature. The flow rate was 50L/h, and the diameter of the resin column was 0.3 m and the height was 3 m. The properties of the ammonium bicarbonate solution after removal of the ammonium alkyl benzene sulfonate are shown in table 2.
TABLE 2
The present invention is not limited to the above-described embodiments, and any variations, modifications, and substitutions which may occur to those skilled in the art may be made without departing from the spirit of the invention.
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| CN1531988A (en) * | 2003-03-25 | 2004-09-29 | 巴斯福股份公司 | Method for purifying or treating ionic liquid by absorption separation |
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| CN107002175A (en) * | 2014-09-24 | 2017-08-01 | 日东电工株式会社 | The adsorption and separation material of rare earth element |
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