CN111606333A - Method for purifying ammonium bicarbonate - Google Patents
Method for purifying ammonium bicarbonate Download PDFInfo
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- CN111606333A CN111606333A CN202010507980.XA CN202010507980A CN111606333A CN 111606333 A CN111606333 A CN 111606333A CN 202010507980 A CN202010507980 A CN 202010507980A CN 111606333 A CN111606333 A CN 111606333A
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- ammonium bicarbonate
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- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 title claims abstract description 79
- 235000012538 ammonium bicarbonate Nutrition 0.000 title claims abstract description 79
- 239000001099 ammonium carbonate Substances 0.000 title claims abstract description 79
- 238000000034 method Methods 0.000 title claims abstract description 38
- 239000011347 resin Substances 0.000 claims abstract description 59
- 229920005989 resin Polymers 0.000 claims abstract description 59
- 239000000243 solution Substances 0.000 claims abstract description 45
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000001179 sorption measurement Methods 0.000 claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- 238000005406 washing Methods 0.000 claims abstract description 15
- 229910001868 water Inorganic materials 0.000 claims abstract description 14
- 238000000746 purification Methods 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 11
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 230000007935 neutral effect Effects 0.000 claims abstract description 8
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims abstract description 6
- 235000019345 sodium thiosulphate Nutrition 0.000 claims abstract description 6
- 238000002791 soaking Methods 0.000 claims abstract description 4
- 238000004140 cleaning Methods 0.000 claims abstract description 3
- 238000004108 freeze drying Methods 0.000 claims abstract description 3
- 238000003795 desorption Methods 0.000 claims description 8
- 230000008929 regeneration Effects 0.000 claims description 8
- 238000011069 regeneration method Methods 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 5
- 238000002386 leaching Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 3
- ZNNZYHKDIALBAK-UHFFFAOYSA-M potassium thiocyanate Chemical compound [K+].[S-]C#N ZNNZYHKDIALBAK-UHFFFAOYSA-M 0.000 claims description 3
- 229940116357 potassium thiocyanate Drugs 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 2
- 238000001953 recrystallisation Methods 0.000 claims description 2
- 239000012452 mother liquor Substances 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 3
- 238000002203 pretreatment Methods 0.000 abstract description 2
- 238000002425 crystallisation Methods 0.000 description 9
- 230000008901 benefit Effects 0.000 description 5
- 230000008025 crystallization Effects 0.000 description 5
- 229960001484 edetic acid Drugs 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 235000010855 food raising agent Nutrition 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 229910017053 inorganic salt Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 241001330002 Bambuseae Species 0.000 description 1
- 206010058467 Lung neoplasm malignant Diseases 0.000 description 1
- 206010033546 Pallor Diseases 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- 238000002479 acid--base titration Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 239000003957 anion exchange resin Substances 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000008429 bread Nutrition 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000007810 chemical reaction solvent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 235000014510 cooky Nutrition 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000015203 fruit juice Nutrition 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 201000005202 lung cancer Diseases 0.000 description 1
- 208000020816 lung neoplasm Diseases 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000000618 nitrogen fertilizer Substances 0.000 description 1
- 230000029553 photosynthesis Effects 0.000 description 1
- 238000010672 photosynthesis Methods 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/26—Carbonates or bicarbonates of ammonium
-
- 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
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/20—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the sorbent material
- B01D15/203—Equilibration or regeneration
-
- 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
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/26—Selective adsorption, e.g. chromatography characterised by the separation mechanism
- B01D15/36—Selective adsorption, e.g. chromatography characterised by the separation mechanism involving ionic interaction
- B01D15/361—Ion-exchange
- B01D15/363—Anion-exchange
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a purification method of ammonium bicarbonate, which adopts D201 resin to prepare an adsorption column, adds an ammonium bicarbonate solution from the upper part of the adsorption column, collects the ammonium bicarbonate solution from the lower part of the adsorption column, and obtains high-purity ammonium bicarbonate through freeze drying. The resin is pretreated, and the pretreatment method comprises the following steps: soaking the resin in deionized water for 24 hours; then treating with NaOH aqueous solution, and cleaning with water after the treatment is finished; then treating the mixture by using a first hydrochloric acid solution, and washing the mixture to be neutral by using clear water; finally, the mixture is treated by sodium thiosulfate and EDTA and washed by clear water to be neutral. The method can effectively solve the problems that the ammonium bicarbonate is easy to decompose and a large amount of ammonium bicarbonate in the purified mother liquor causes raw material waste, is quick, environment-friendly and free of secondary pollution, and the purity of the prepared ammonium bicarbonate is up to more than 99.9 percent, and is simple and easy to operate and environment-friendly.
Description
Technical Field
The invention relates to the technical field of inorganic salt purification, in particular to a method for purifying ammonium bicarbonate.
Background
Ammonium bicarbonate (NH)4HCO3) Also called ammonium bicarbonate, is a white monoclinic or orthorhombic crystal system crystal with a molecular weight of 79.1 and a theoretical nitrogen content of 17.72 percent, and is an inorganic salt with wide application. Can be used as a nitrogen fertilizer in agriculture, is suitable for various soils, can simultaneously provide ammonium nitrogen and carbon dioxide required by the growth of crops, can promote the growth and photosynthesis of the crops, promote the seedlings and grow leaves, and can be used as a top dressing and a base fertilizer for direct application. Can be used as high-grade leavening agent in food, and can be used as leavening agent for bread, cookies, battercake, etc. in combination with sodium bicarbonate, and also used as raw material of foaming powder fruit juice, and used for blanching green vegetables, bamboo shoot, etc. And medicines and reagents, and the fermentation powder also takes the product as a main component and is matched with an acidic substance. In pharmaceutical applicationsIn addition, the introduction of ammonium bicarbonate can improve the distribution proportion of HPCT, prolong the retention time of the medicine in lung, improve the curative effect of HPCT on lung cancer and the like. The current environments of various industries all require that ammonium bicarbonate series products continuously explore new processing techniques and novel ammonium bicarbonate products to adapt to the standards of corresponding industries while taking the inherent value of the ammonium bicarbonate series products into consideration and stabilizing the market status of the ammonium bicarbonate series products. In order to better meet the requirements of more fields, the purity of the ammonium bicarbonate is required to be improved.
Currently, ammonium bicarbonate is mainly prepared by a crystallization method, and ammonium bicarbonate is separated out from a solution by utilizing solubility difference. However, the crystallization method for preparing ammonium bicarbonate has the following disadvantages: 1. in the crystallization process, the loss amount of ammonium bicarbonate is large, and a large amount of ammonium bicarbonate is contained in the mother liquor, so that waste is easily caused. 2. Because the ammonium bicarbonate is decomposed into carbon dioxide, ammonia and water at the temperature of over 36 ℃, the ammonium bicarbonate can be completely decomposed at the temperature of 60 ℃, the temperature is high in the crystallization process, the separated ammonium bicarbonate is easy to decompose, the yield of the ammonium bicarbonate is reduced, the preparation cost of the ammonium bicarbonate is high, and the industrial production is not facilitated. 3. The ammonium bicarbonate purified by the crystallization method contains impurities such as metal ions, and is difficult to remove from the ammonium bicarbonate formed by the crystallization, so that the purity of the ammonium bicarbonate is not high.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to solve the problems that the mother liquor after crystallization contains a large amount of ammonium bicarbonate, the mother liquor is difficult to be completely utilized, the crystallization temperature is high, and the ammonium bicarbonate is easy to decompose in the conventional crystallization method for preparing the ammonium bicarbonate, and provides a method for purifying the ammonium bicarbonate.
In order to solve the technical problems, the invention adopts the following technical scheme:
a process for purifying ammonium hydrogen carbonate includes such steps as preparing adsorption column with D201 resin, adding ammonium hydrogen carbonate solution from the top of adsorption column, collecting the ammonium hydrogen carbonate solution from the bottom of adsorption column, and freeze drying.
Wherein, the resin is pretreated, and the pretreatment method comprises the following steps: soaking the resin in deionized water for 24 hours; then treating with NaOH aqueous solution, and cleaning with water after the treatment is finished; then treating the mixture by using a first hydrochloric acid solution, and washing the mixture to be neutral by using clear water; and finally, treating the mixture for 0.5 to 10 hours by using a mixed solution of sodium thiosulfate and EDTA (ethylene diamine tetraacetic acid), and washing the mixture to be neutral by using clear water.
Further, the concentration of the NaOH aqueous solution is 1% -5%, the treatment volume is 5-10 times of the volume of the resin, and then the resin is cleaned by deionized water of 10-20 times.
Further, the concentration of the first hydrochloric acid solution is 0.5-8%, and the treatment volume is 5-10 times of the volume of the resin.
Furthermore, the dosage of the sodium thiosulfate accounts for 1-20% of the mass of the resin, and the dosage of the EDTA accounts for 0.5-25% of the mass of the resin.
Further, the content of ammonium bicarbonate in the added ammonium bicarbonate solution is 99.4-99.5%, and the leaching solution outflow rate is 30-100 mL/h.
Further, still include the desorption regeneration process of adsorption column, desorption regeneration process is: and adding a second hydrochloric acid solution from the upper part of the adsorption column for washing, wherein the adding speed of the second hydrochloric acid solution is consistent with the speed of the ammonium bicarbonate solution during adsorption until the effluent liquid is not red when being detected by a potassium thiocyanate solution after being acidified, and then washing by distilled water, so that the adsorption material is regenerated.
Further, the concentration of the second hydrochloric acid solution is 0.1-5 mol/L, the using amount of the second hydrochloric acid solution is 2-5 times of the volume of the resin, and the treatment time is 1-10 hours.
Further, the washing amount of the distilled water is 3-5 times of the volume of the resin.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention adopts a resin adsorption mode to purify ammonium bicarbonate, and adopts pretreated D201 resin to prepare an adsorption column. D201 is styrene-divinylbenzene copolymer with macroporous structure and quaternary ammonium group [ -N (CH)3)3OH]The anion exchange resin of (4) is capable of adsorbing a plurality of ions (mainly comprising Fe) in the ammonium bicarbonate solution2+And Fe3+) Therefore, the ammonium bicarbonate solution can be purified, and has the advantages of difficult poisoning, high exchange speed,The stability is good. Effectively solves the problems that the ammonium bicarbonate is easy to decompose and a large amount of ammonium bicarbonate in the mother liquor after purification causes waste of raw materials.
2. The invention carries out adsorption purification by utilizing the pretreated resin, and has the advantages of high efficiency, simple operation, easily obtained materials and recyclable materials. In the conventional purification method in the prior art, such as a recrystallization method, the purity of the purified ammonium bicarbonate is 99.4-99.5%, but the purification method provided by the invention has high economic benefit, the purity of the prepared ammonium bicarbonate is more than 99.94%, and the method is simple and easy to operate, green and environment-friendly.
3. The invention also provides a step of desorption regeneration of the resin, and the resin after adsorption is saturated and can be regenerated by treatment of hydrochloric acid solution, so that the resin can be recycled, the purification cost of ammonium bicarbonate is reduced, and the method is suitable for industrial production.
Drawings
FIG. 1 is a process flow diagram of a purification method of ammonium bicarbonate of the present invention.
Detailed Description
The invention will be further explained with reference to the drawings and the embodiments.
Example 1
A method for purifying ammonium bicarbonate, see fig. 1, comprising the steps of:
(1) d201 resin pretreatment: soaking the resin in deionized water for 24 hr to remove impurities (pore-forming agent, catalyst, reaction solvent, etc.) generated during production; after being treated by 4 percent NaOH aqueous solution with the volume 5-10 times of that of the resin, the resin is washed by 10-20 times of that of the resin, then treated by 4 percent hydrochloric acid solution with the volume 5-10 times of that of the resin, and washed to be neutral by clear water; and finally, treating the resin for 0.5h by using 1% of sodium thiosulfate and 0.5% of EDTA according to the mass of the resin, and washing the resin to be neutral by using clear water to obtain the treated D201 resin.
(2) And (3) purifying ammonium bicarbonate: and weighing about 80g of the pretreated D201 resin, and filling the D201 resin into an adsorption column with the column height of about 10cm to obtain the D201 resin adsorption column. Adding the prepared ammonium bicarbonate solution from the upper part of the adsorption column, adjusting the speed of the leaching solution to 60 mL/h, collecting 300mL of the leaching solution at the lower part, and carrying out freeze vacuum drying on the leaching solution for 12h to obtain the ammonium bicarbonate.
The purity of the original ammonium bicarbonate is 99.4 percent, and the purity of the ammonium bicarbonate is 99.960 percent by adopting an acid-base titration method to detect the purity of the ammonium bicarbonate.
Example 2
The difference from the embodiment 1 is that the original purity of the ammonium bicarbonate in the embodiment 2 is 95-96%, and the rest steps are the same as the embodiment 1, so that the purity of the purified ammonium bicarbonate is obtained.
Example 3
The difference from example 1 is that the flow rate of ammonium bicarbonate in example 3 is 30mL/h, and the remaining steps are the same as example 1, thus obtaining the purity of purified ammonium bicarbonate.
Example 4
The difference from the embodiment 1 is that the pretreatment process of the D201 resin in the embodiment 4 is different, and the rest steps are the same as the embodiment 1, so that the purity of the purified ammonium bicarbonate is obtained. The method in this example can be used without EDTA.
In this example, the pretreatment process for D201 is as follows:
repeatedly washing new resin with deionized water for 8 times, and slowly flowing through the resin with 1mol/L HCl, wherein the use amount of the resin is 4 times that of the resin; after rinsing with water until the effluent pH = about 5, the resin was flowed through with 3 bed volumes of NaCl (5%) solution; then NaOH (1 mol/L) solution with the bed volume of 4 times is used for treating the resin; washing with water until the pH of the effluent is about = 9; HCl (1 mol/L) with 4 times bed volume flows through the resin, and the dosage is 4 times of the resin; finally rinsed with deionized water to an effluent pH > 6. All flow rates were 1.5 bed volumes per hour.
The main parameters in examples 1-4 are shown in the following table.
Example 5: d201, desorption and regeneration of the resin adsorption column:
adding 1mol/L hydrochloric acid solution with the volume 2 times of the resin volume from the upper part of the adsorption column for washing until the effluent liquid is not red by using potassium thiocyanate solution after being acidified. And then washing with distilled water with the volume 3-5 times of the volume of the resin, and keeping the eluent velocity consistent with the velocity during the adsorption operation to obtain the D201 resin adsorption column regenerated by desorption.
Example 6: repeated adsorption of D201 resin adsorption column
The desorbed and regenerated D201 resin adsorption column of example 5 is used again for purifying ammonium bicarbonate. The purification conditions were the same as in example 1, namely, the prepared ammonium bicarbonate solution was added from above the adsorption column, the velocity of the extract was adjusted to 60 mL/h, 300mL of the extract was collected, and after vacuum-drying at-75 ℃ for 12h, the purity was measured. The adsorption column of D201 resin was then desorbed and regenerated by the method of example 5, and then purified again. Repeating for 7 times to obtain the ammonium bicarbonate with the purity respectively as follows: 99.952%, 99.940%, 99.935%, 99.928%, 99.910%, 99.905% and 99.895% of the material, and the purity is only reduced by 0.065%, which shows that the material has extremely high regeneration performance.
Therefore, the purification method provided by the invention has high economic benefit, and the purity of the prepared ammonium bicarbonate is as high as more than 99.9%. The D201 resin adsorption column is repeatedly used for 7 times after desorption treatment, the purity is only reduced by 0.065 percent, and the material has extremely high regeneration performance, has the advantages of simple and easy operation, environmental protection, greatly reduces the purification cost of the ammonium bicarbonate, and is suitable for being popularized and used in factories.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the technical solutions, and those skilled in the art should understand that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions, and all that should be covered by the claims of the present invention.
Claims (9)
1. A method for purifying ammonium bicarbonate is characterized in that D201 resin is adopted to prepare an adsorption column, an ammonium bicarbonate solution is added from the upper part of the adsorption column, the ammonium bicarbonate solution below the adsorption column is collected, and freeze drying is carried out to obtain high-purity ammonium bicarbonate.
2. The method for purifying ammonium bicarbonate according to claim 1, wherein the resin is pretreated by: soaking the resin in deionized water for 24 hours; then treating with NaOH aqueous solution, and cleaning with water after the treatment is finished; then treating the mixture by using a first hydrochloric acid solution, and washing the mixture to be neutral by using clear water; and finally, treating the mixture for 0.5 to 10 hours by using a mixed solution of sodium thiosulfate and EDTA, and washing the mixture to be neutral by using clear water.
3. The method for purifying ammonium bicarbonate according to claim 2, wherein the concentration of the NaOH aqueous solution is 1-5%, the treatment volume is 5-10 times of the resin volume, and the resin is washed with 10-20 times of deionized water.
4. The method of claim 2, wherein the concentration of the first hydrochloric acid solution is 0.5% to 8%, and the treatment volume is 5 to 10 times the resin volume.
5. The method for purifying ammonium bicarbonate according to claim 2, wherein the amount of the sodium thiosulfate is 1% to 20% of the mass of the resin, and the amount of the EDTA is 0.5% to 25% of the mass of the resin.
6. The method for purifying ammonium bicarbonate according to claim 1, wherein the ammonium bicarbonate content in the added ammonium bicarbonate solution is 99.4-99.5%, the ammonium bicarbonate cannot be purified to 99.9% by a conventional purification method such as recrystallization, and the leaching solution outflow rate is 30-100 mL/h.
7. The method for purifying ammonium bicarbonate according to any one of claims 1 to 6, further comprising a desorption regeneration process of the adsorption column, wherein the desorption regeneration process comprises the following steps: and adding a second hydrochloric acid solution from the upper part of the adsorption column for washing, wherein the adding speed of the second hydrochloric acid solution is consistent with the speed of the ammonium bicarbonate solution during adsorption until the effluent liquid is not red when being detected by a potassium thiocyanate solution after being acidified, and then washing by distilled water, so that the adsorption material is regenerated.
8. The method for purifying ammonium bicarbonate according to claim 7, wherein the concentration of the second hydrochloric acid solution is 0.1-5 mol/L, the amount of the second hydrochloric acid solution is 2-5 times of the volume of the resin, and the treatment time is 1-10 h.
9. The method for purifying ammonium bicarbonate according to claim 7, wherein the amount of the distilled water is 3 to 5 times of the volume of the resin.
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|---|---|---|---|---|
| DE502675C (en) * | 1926-05-28 | 1930-07-14 | Kohlentechnik M B H Ges | Method for purifying ammonium bicarbonate |
| EP0146512A1 (en) * | 1983-11-15 | 1985-06-26 | Swedspan Ab | A suspension of ammonium carbonate and/or ammonium hydrogen carbonate of improved stability and its use |
| CN1761617A (en) * | 2003-02-11 | 2006-04-19 | 航空工业矿石公司 | Method for recovering purified sodium bicarbonate and ammonium sulfate |
| CN108383139A (en) * | 2018-04-20 | 2018-08-10 | 包头市远达鑫化工有限公司 | The process units and method of ammonium hydrogen carbonate |
| US20190071338A1 (en) * | 2015-01-14 | 2019-03-07 | Bion Environmental Technologies, Inc. | Process to recover ammonium bicarbonate from wastewater |
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2020
- 2020-06-05 CN CN202010507980.XA patent/CN111606333A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE502675C (en) * | 1926-05-28 | 1930-07-14 | Kohlentechnik M B H Ges | Method for purifying ammonium bicarbonate |
| EP0146512A1 (en) * | 1983-11-15 | 1985-06-26 | Swedspan Ab | A suspension of ammonium carbonate and/or ammonium hydrogen carbonate of improved stability and its use |
| CN1761617A (en) * | 2003-02-11 | 2006-04-19 | 航空工业矿石公司 | Method for recovering purified sodium bicarbonate and ammonium sulfate |
| US20190071338A1 (en) * | 2015-01-14 | 2019-03-07 | Bion Environmental Technologies, Inc. | Process to recover ammonium bicarbonate from wastewater |
| CN108383139A (en) * | 2018-04-20 | 2018-08-10 | 包头市远达鑫化工有限公司 | The process units and method of ammonium hydrogen carbonate |
Non-Patent Citations (3)
| Title |
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