CN101597069A - A kind of purification process of ammonia - Google Patents
A kind of purification process of ammonia Download PDFInfo
- Publication number
- CN101597069A CN101597069A CNA2009101002910A CN200910100291A CN101597069A CN 101597069 A CN101597069 A CN 101597069A CN A2009101002910 A CNA2009101002910 A CN A2009101002910A CN 200910100291 A CN200910100291 A CN 200910100291A CN 101597069 A CN101597069 A CN 101597069A
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- Prior art keywords
- ammonia
- magnesium chloride
- ammoniate
- gas
- hex
- Prior art date
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 154
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 73
- 238000000746 purification Methods 0.000 title claims abstract description 25
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims abstract description 94
- 239000007789 gas Substances 0.000 claims abstract description 67
- 229960002337 magnesium chloride Drugs 0.000 claims abstract description 32
- 229910001629 magnesium chloride Inorganic materials 0.000 claims abstract description 32
- 229940073589 magnesium chloride anhydrous Drugs 0.000 claims abstract description 30
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 26
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000001301 oxygen Substances 0.000 claims abstract description 16
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000001257 hydrogen Substances 0.000 claims abstract description 14
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 14
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052786 argon Inorganic materials 0.000 claims abstract description 13
- 229910002091 carbon monoxide Inorganic materials 0.000 claims abstract description 13
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 230000002441 reversible effect Effects 0.000 claims abstract description 5
- 238000010521 absorption reaction Methods 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims description 7
- 238000007711 solidification Methods 0.000 claims description 2
- 230000008023 solidification Effects 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 9
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 230000000274 adsorptive effect Effects 0.000 abstract description 4
- 239000002808 molecular sieve Substances 0.000 abstract description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002594 sorbent Substances 0.000 abstract description 2
- 238000004587 chromatography analysis Methods 0.000 description 10
- 238000005070 sampling Methods 0.000 description 10
- 238000010586 diagram Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000003814 drug Substances 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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Abstract
The invention discloses a kind of purification process of ammonia.This purification process is based on Magnesium Chloride Anhydrous and inhales ammonia and generate magnesium chloride hex-ammoniate, magnesium chloride hex-ammoniate and be heated and put this reversible reaction of ammonia, the ammonia of ammonia mixed gas is generated magnesium chloride hex-ammoniate by Magnesium Chloride Anhydrous absorption, and oxygen, nitrogen, argon gas, hydrogen or carbon monoxide can not be adsorbed, still exist with gaseous state, thereby reach ammonia and the isolating purpose of foreign gas.At present industrial purification process technology commonly used and equipment more complicated generally are fit to scale operation, can not be flexibly, mobile carries and discrete production.And the present invention to adopt cheap Magnesium Chloride Anhydrous be sorbent material, equipment is fairly simple, only needs a reaction vessel of being furnished with heating member and valve, can flexibly, flexibly transport and realize discrete production.And the theoretical ammonia adsorptive capacity of Magnesium Chloride Anhydrous reaches about 100%, far surpasses the adsorptive capacity of molecular sieve.Adopt the method purifying ammonia among the present invention, can reduce cost greatly.
Description
Technical field
The present invention relates to a kind of purification process of ammonia.
Background technology
Ammonia (chemical formula: NH
3) be a kind of important chemical material gas, have extensive use, can be used for producing liquefied ammonia, ammoniacal liquor, nitric acid, urea, ammonium salt, plastics, dyestuff, pharmaceuticals, synthon, plastics and dyestuff etc.In recent years, ammonia as a kind of important electron gas in semiconductor industry application also more and more widely.Simultaneously, ammonia also can be used as the cooling agent of new type compressor.Along with the development of technology and deepening continuously of ammonia application, industry member, research circle have proposed more and more higher requirement to the purity of ammonia, particularly at semi-conductor and field of medicaments, require to use high purity ammonia gas.Therefore, ammonia purity has decisive role to the quality and the added value of its product, and the ammonia that production purity is high is the developing direction of ammonia synthesizing industry.
In decades, constantly development is with progressive for the ammonia purifying process, and new purifying process continues to bring out, and ammonia purification process commonly used at present mainly comprises: pressure swing adsorption process, rectification method, chemical absorption method and membrane separation process etc.These methods have the relative merits of self, and development of new, ammonia purification process and technology are still important problem of ammonia industry efficiently.
Summary of the invention
The purification process that the purpose of this invention is to provide a kind of ammonia is inhaled ammonia based on Magnesium Chloride Anhydrous and is generated magnesium chloride hex-ammoniate, and magnesium chloride hex-ammoniate is heated and puts this reversible reaction of ammonia and carry out purifying.
The technical solution used in the present invention is:
This purification process is based on Magnesium Chloride Anhydrous and inhales ammonia and generate magnesium chloride hex-ammoniate, magnesium chloride hex-ammoniate and be heated and put this reversible reaction of ammonia, the ammonia of ammonia mixed gas is generated magnesium chloride hex-ammoniate by the Magnesium Chloride Anhydrous absorption solidification, and oxygen, nitrogen, argon gas, hydrogen or carbon monoxide can not be adsorbed by it, still exist with gaseous state, after residual gas can being extracted, allow magnesium chloride hex-ammoniate be subjected to the ammonia of heat release purifying.
Concrete steps are as follows:
1) content there is the ammonia gas mixture body of oxygen, nitrogen, argon gas, hydrogen or carbon monoxide do processed;
2) under the room temperature above-mentioned ammonia gas mixture body fed and be equipped with in the container of excessive Magnesium Chloride Anhydrous, treat that ammonia is absorbed by Magnesium Chloride Anhydrous and is solidified into magnesium chloride hex-ammoniate, and oxygen, nitrogen, argon gas, hydrogen or carbon monoxide exist with gaseous state still;
3) by vacuum pump with oxygen, nitrogen, argon gas, hydrogen or carbon monoxide removal remaining in the container after;
4) under 150 ℃～600 ℃ temperature, heat, allow it emit the ammonia of purifying to magnesium chloride hex-ammoniate.
The beneficial effect that the present invention has is:
Magnesium Chloride Anhydrous can with ammonia generation chemical reaction, generate solid-state magnesium chloride hex-ammoniate, molecular formula is MgCl
26NH
3, heating get back behind the magnesium chloride hex-ammoniate Magnesium Chloride Anhydrous and ammonia, are put ammonia at the suction that so can circulate.Simultaneously, Magnesium Chloride Anhydrous can not adsorption of oxygen, gas such as nitrogen, argon gas, hydrogen or carbon monoxide.The present invention utilizes the selective adsorption of Magnesium Chloride Anhydrous and reversible cycle to inhale, put the ammonia characteristic, is the ammonia purification process of carrier based on Magnesium Chloride Anhydrous and ammonia complex magnesium chloride hex-ammoniate thereof.This method is solidificated in the ammonia in the ammonia mixed gas in the magnesium chloride hex-ammoniate, and foreign gas still exists with gaseous form, reaches effective isolating purpose with this.At last, solidified ammonia is discharged, obtain the ammonia of purifying by the heating magnesium chloride hex-ammoniate.
At present industrial purification process technology commonly used and equipment more complicated generally are fit to scale operation, can not be flexibly, mobile carries and discrete production.And the cheap Magnesium Chloride Anhydrous of purification process employing disclosed by the invention is a sorbent material, and equipment is fairly simple, only needs a reaction vessel of being furnished with heating member and valve, can flexibly, flexibly transport and realize discrete production.And the theoretical ammonia adsorptive capacity of Magnesium Chloride Anhydrous that adopts of the present invention reaches about 100%, far surpasses the adsorptive capacity of molecular sieve.Therefore, adopt the method purifying ammonia among the present invention, can reduce cost greatly.
Description of drawings
Fig. 1 is the gas chromatogram of gas before and after purifying among the embodiment 1; (a) before the purification, (b) after the purification.
Fig. 2 is the gas chromatogram of gas before and after purifying among the embodiment 2; (a) before the purification, (b) after the purification.
Fig. 3 is the gas chromatogram of gas before and after purifying among the embodiment 3; (a) before the purification, (b) after the purification.
Embodiment
Embodiment 1:
The ammonia that will contain oxygen is after processed, and gas chromatographic analysis is carried out in gas sampling, and Fig. 1 (a) is the gas chromatogram of gas before corresponding the purification.Then, mixed gas after at room temperature will dewatering feeds and is equipped with in the container of excessive Magnesium Chloride Anhydrous, treat that ammonia is absorbed by Magnesium Chloride Anhydrous and is solidified into magnesium chloride hex-ammoniate, and oxygen exists with gaseous state still.After by vacuum pump the residual gas in the container being removed, give magnesium chloride hex-ammoniate, emit the ammonia of purifying 150 ℃ of heating down.Sub-sampling carries out gas chromatographic analysis again, and Fig. 1 (b) is the gas chromatogram after purifying.By comparison diagram 1 (a) and (b) as can be known, the content of foreign gas oxygen drops to 0.5737% by original 50.7599%, and the purity of ammonia improves greatly.As seen, employing the present invention can effectively remove the oxygen in the ammonia gas mixture.
Embodiment 2:
The ammonia that will contain nitrogen is after processed, and gas chromatographic analysis is carried out in gas sampling, and Fig. 2 (a) is the gas chromatogram of gas before corresponding the purification.Then, mixed gas after at room temperature will dewatering feeds and is equipped with in the container of excessive Magnesium Chloride Anhydrous, treat that ammonia is absorbed by Magnesium Chloride Anhydrous and is solidified into magnesium chloride hex-ammoniate, and nitrogen exists with gaseous state still.After by vacuum pump the residual gas in the container being removed, give magnesium chloride hex-ammoniate, emit the ammonia of purifying 200 ℃ of heating down.Sub-sampling carries out gas chromatographic analysis again, and Fig. 2 (b) is the gas chromatogram after purifying.By comparison diagram 2 (a) and (b) as can be known, the content of foreign gas oxygen drops to 0.5974% by original 24.7809%, and the purity of ammonia improves greatly.As seen, employing the present invention can effectively remove the nitrogen in the ammonia gas mixture.
Embodiment 3:
The ammonia that will contain argon gas is after processed, and gas chromatographic analysis is carried out in gas sampling, and Fig. 3 (a) is the gas chromatogram of gas before corresponding the purification.Then, mixed gas after at room temperature will dewatering feeds and is equipped with in the container of excessive Magnesium Chloride Anhydrous, treat that ammonia is absorbed by Magnesium Chloride Anhydrous and is solidified into magnesium chloride hex-ammoniate, and argon gas exists with gaseous state still.After by vacuum pump the residual gas in the container being removed, give magnesium chloride hex-ammoniate, emit the ammonia of purifying 250 ℃ of heating down.Sub-sampling carries out gas chromatographic analysis again, and Fig. 3 (b) is the gas chromatogram after purifying.By comparison diagram 3 (a) and (b) as can be known, the content of foreign gas oxygen drops to 0.6855% by original 12.6076%, and the purity of ammonia improves greatly.As seen, employing the present invention can effectively remove the argon gas in the ammonia gas mixture.
Embodiment 4:
The ammonia that will contain hydrogen is after processed, and gas chromatographic analysis is carried out in gas sampling.Then, mixed gas after at room temperature will dewatering feeds and is equipped with in the container of excessive Magnesium Chloride Anhydrous, treat that ammonia is absorbed by Magnesium Chloride Anhydrous and is solidified into magnesium chloride hex-ammoniate, and hydrogen exists with gaseous state still.After by vacuum pump the foreign gas hydrogen in the container being removed, give magnesium chloride hex-ammoniate, emit the ammonia of purifying 300 ℃ of heating down.Sub-sampling carries out gas chromatographic analysis again.Find that at last the content of hydrogen has reduced nearly 100 times.
Embodiment 5:
The ammonia that will contain carbon monoxide is after processed, and gas chromatographic analysis is carried out in gas sampling.Then, mixed gas after at room temperature will dewatering feeds and is equipped with in the container of excessive Magnesium Chloride Anhydrous, treat that ammonia is absorbed by Magnesium Chloride Anhydrous and is solidified into magnesium chloride hex-ammoniate, and carbon monoxide exists with gaseous state still.After by vacuum pump the residual gas in the container being removed, give magnesium chloride hex-ammoniate, emit the ammonia of purifying 600 ℃ of heating down.Sub-sampling carries out gas chromatographic analysis again.Find that at last the content of carbon monoxide has also reduced nearly 100 times.
Claims (2)
1, a kind of purification process of ammonia, it is characterized in that: this purification process is based on Magnesium Chloride Anhydrous and inhales ammonia and generate magnesium chloride hex-ammoniate, magnesium chloride hex-ammoniate and be heated and put this reversible reaction of ammonia, the ammonia of ammonia mixed gas is generated magnesium chloride hex-ammoniate by the Magnesium Chloride Anhydrous absorption solidification, and oxygen, nitrogen, argon gas, hydrogen or carbon monoxide can not be adsorbed by it, still exist with gaseous state, after residual gas can being extracted, allow magnesium chloride hex-ammoniate be subjected to the ammonia of heat release purifying.
2, the purification process of a kind of ammonia according to claim 1 is characterized in that concrete steps are as follows:
1) content there is the ammonia gas mixture body of oxygen, nitrogen, argon gas, hydrogen or carbon monoxide do processed;
2) under the room temperature above-mentioned ammonia gas mixture body fed and be equipped with in the container of excessive Magnesium Chloride Anhydrous, treat that ammonia is absorbed by Magnesium Chloride Anhydrous and is solidified into magnesium chloride hex-ammoniate, and oxygen, nitrogen, argon gas, hydrogen or carbon monoxide exist with gaseous state still;
3) by vacuum pump with oxygen, nitrogen, argon gas, hydrogen or carbon monoxide removal remaining in the container after;
4) under 150 ℃～600 ℃ temperature, heat, allow it emit the ammonia of purifying to magnesium chloride hex-ammoniate.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009101002910A CN101597069A (en) | 2009-06-29 | 2009-06-29 | A kind of purification process of ammonia |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009101002910A CN101597069A (en) | 2009-06-29 | 2009-06-29 | A kind of purification process of ammonia |
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| Publication Number | Publication Date |
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| CN101597069A true CN101597069A (en) | 2009-12-09 |
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| CNA2009101002910A Pending CN101597069A (en) | 2009-06-29 | 2009-06-29 | A kind of purification process of ammonia |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113058377A (en) * | 2020-01-02 | 2021-07-02 | 吉林卓创新材料有限公司 | Carbon monoxide tail gas purification method |
-
2009
- 2009-06-29 CN CNA2009101002910A patent/CN101597069A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113058377A (en) * | 2020-01-02 | 2021-07-02 | 吉林卓创新材料有限公司 | Carbon monoxide tail gas purification method |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20091209 |