CN103933934A - Adsorbent for removing trace moisture in gas and preparation method thereof - Google Patents
Adsorbent for removing trace moisture in gas and preparation method thereof Download PDFInfo
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- CN103933934A CN103933934A CN201410191434.4A CN201410191434A CN103933934A CN 103933934 A CN103933934 A CN 103933934A CN 201410191434 A CN201410191434 A CN 201410191434A CN 103933934 A CN103933934 A CN 103933934A
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- molecular sieve
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 80
- 238000002360 preparation method Methods 0.000 title claims description 18
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000002808 molecular sieve Substances 0.000 claims abstract description 46
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims abstract description 28
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 12
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims abstract description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 46
- 239000008367 deionised water Substances 0.000 claims description 22
- 229910021641 deionized water Inorganic materials 0.000 claims description 22
- 238000005406 washing Methods 0.000 claims description 22
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 claims description 18
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 18
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 18
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 claims description 18
- 229910002651 NO3 Inorganic materials 0.000 claims description 10
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 10
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- 239000004411 aluminium Substances 0.000 claims description 3
- 230000004048 modification Effects 0.000 claims description 3
- 238000012986 modification Methods 0.000 claims description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 2
- 229910052788 barium Inorganic materials 0.000 claims description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 239000011575 calcium Substances 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 claims description 2
- 229910052712 strontium Inorganic materials 0.000 claims description 2
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 2
- 230000018044 dehydration Effects 0.000 abstract description 28
- 238000006297 dehydration reaction Methods 0.000 abstract description 28
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 229910052684 Cerium Inorganic materials 0.000 abstract description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 abstract description 2
- 230000008929 regeneration Effects 0.000 abstract description 2
- 238000011069 regeneration method Methods 0.000 abstract description 2
- 229910001964 alkaline earth metal nitrate Inorganic materials 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- 150000003839 salts Chemical class 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 76
- 238000002474 experimental method Methods 0.000 description 43
- 238000005259 measurement Methods 0.000 description 21
- 239000011259 mixed solution Substances 0.000 description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 16
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 229910021529 ammonia Inorganic materials 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 4
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 3
- 229910001882 dioxygen Inorganic materials 0.000 description 3
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 2
- 229910021536 Zeolite Inorganic materials 0.000 description 2
- -1 alkaline earth metal cation Chemical class 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910001415 sodium ion Inorganic materials 0.000 description 2
- 239000010457 zeolite Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 description 1
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses an adsorbent for removing trace moisture in gas. The adsorbent has the advantages of high dehydration depth, large adsorption quantity, low cost and good regeneration performance. The adsorbent for removing trace moisture in gas is prepared by a method for modifying a molecular sieve by using a metal salt consisting of cerium nitrate, aluminum nitrate and other alkaline earth metal nitrates, wherein the mass percent of cerium element, aluminum element and other alkaline earth metal elements is 0.02-10%, 0.05-3% and 0.08-10% respectively based on the total mass of the modified molecular sieve.
Description
Technical field
The present invention relates to adsorbent and preparation method, be specifically related to a kind of for removing adsorbent and the preparation method of gas micro-moisture.
Background technology
In recent years, electronic industry has become one of global maximum industry.In the production of electronic devices and components, mainly serve as the preparation of protecting gas, reaction gas and taking sparkling ultra-pure gas and also suddenly become heat subject.In order to prepare in the unstripped gas of ultra-pure gas, often contain miscellaneous impurity, wherein micro-moisture is large and to remove difficulty be maximum compared with other impurity for the impact of device, therefore how to remove the large difficult point that micro-moisture in gas becomes the ultra-pure gas of preparation.
In prior art in gas the removal methods of micro-moisture mainly with rectifying be adsorbed as master.Wherein, often operating condition is comparatively gentle, equipment is relatively simple, cost of investment is lower, in many cases, can obtain the water content lower than other technologies, and energy consumption is lower, has become the main method that removes minor amount of water in gas for absorption method.
Although absorption method has plurality of advantages, but due to the simultaneous desorption process of absorption, use conventional adsorbent often to have the problem of dehydration degree of depth deficiency, for example, publication number is US2002074289A1, the United States Patent (USP) that name is called " Method for purifying semiconductor gases " discloses use 3A molecular sieve as deep dehydration adsorbent, and its weak point is finally can only be by moisture removal in gas to 100ppb, and cannot reach the higher degree of depth; And for example, publication number is CN1089884, the Chinese patent that name is called " a kind of colour changeable dewatering agent and preparation method thereof " discloses with silver salt modification 4A molecular sieve does deep dehydration agent, its weak point is finally also can only, by moisture removal in gas to 100ppb, far cannot reach the demand of industrial production of ultra-pure gas.
Summary of the invention
The object of the invention is to solve defect and the problem that prior art exists, provide a kind of for removing the adsorbent of gas micro-moisture.This adsorbent dehydration degree of depth is high, adsorbance is large, cost is low, regenerability is good.
The present invention also provides the preparation method of above-mentioned adsorbent, and the method step is simple, is easy to control, and it is convenient to implement; The application of above-mentioned adsorbent is also provided in addition; The method that adopts above-mentioned adsorbent to remove micro-moisture in high-purity gas is provided.
The technical scheme that the present invention realizes above-mentioned purpose is as follows:
Of the present invention for removing the adsorbent of gas micro-moisture, it is that the method for the slaine modified molecular screen by being comprised of cerous nitrate, aluminum nitrate and other alkaline earth nitrate makes, the gross mass of molecular sieve after modification of take is benchmark, Ce elements mass percent is 0.02～10%, aluminium element mass percent is 0.05～3%, and other alkali earth metal mass percent is 0.08～10%.
Of the present invention for removing the adsorbent of gas micro-moisture, its further technical scheme is that other described alkaline earth nitrate is one or more in magnesium nitrate, calcium nitrate, strontium nitrate and barium nitrate; Other described alkaline-earth metal is one or more in magnesium, calcium, strontium and barium.
Of the present invention for removing the adsorbent of gas micro-moisture, its further technical scheme can also be that described molecular sieve is 13X molecular sieve or 4A molecular sieve.
Of the present invention above-mentioned for removing the preparation method of the adsorbent of gas micro-moisture, it comprises the following steps: cerous nitrate, aluminum nitrate and other alkaline earth nitrate are dissolved in and in deionized water, form solution, after adding molecular sieve dipping 6～24h under normal temperature, filter, washing, by the sample obtaining roasting 4～8h at 350～400 ℃, obtain for removing the adsorbent of gas micro-moisture.
Of the present invention for removing the preparation method of the adsorbent of gas micro-moisture, its further technical scheme is that the described cerous nitrate concentration in solution is 0.05～0.5mol/L, the concentration of aluminum nitrate in solution is 0.05～0.5mol/L, the concentration of other alkaline earth nitrate in solution is 0.05～0.5mol/L, and solution quality is 10～20 times of molecular sieve quality.
Of the present invention for removing the preparation method of the adsorbent of gas micro-moisture, its further technical scheme can also be that other described alkaline earth nitrate is one or more in magnesium nitrate, calcium nitrate, strontium nitrate and barium nitrate.
Of the present invention for removing the preparation method of the adsorbent of gas micro-moisture, its further technical scheme can also be that described molecular sieve is 13X molecular sieve or 4A molecular sieve.
Of the present invention can the application in micro-moisture in removing gas for removing the adsorbent of gas micro-moisture.Be preferred for removing high-purity N
2, high-purity O
2, high-purity H
2, high-purity N H
3, high-purity CH
4, high-purity C
2h
4or micro-moisture in rare gas.
The present invention adopts above-mentioned adsorbent to remove the method for micro-moisture in gas, comprise the following steps: adsorbent roasting 4～8h at 350～400 ℃ is activated, then use high-purity gas for unstripped gas, at normal temperature, pressure is under 0.1～0.3MPa, to carry out dynamically water suction experiment, uses moisture monitor measurement result.
Compared with prior art the present invention has following beneficial effect:
It is raw material that adsorbent of the present invention adopts zeolite molecular sieve, and price is comparatively cheap, has effectively reduced the preparation cost of adsorbent; This adsorbent is in zeolite molecular sieve, to introduce cerium, aluminium and other alkaline earth metal cation to strengthen absorption property, because hydrone is polar molecule, and above-mentioned cationic charge radius compares the charge radius of sodium ion than large (the charge radius ratio that aluminum ions charge radius compares sodium ion exceeds more than 5 times), there is stronger polarizability, thereby strengthened the interaction with hydrone, increased the adsorption capacity to water, so this preparation method can effectively change the characterization of adsorption of molecular sieve, can improve significantly its dehydration degree of depth and adsorbance; This adsorbent can continue to use after regeneration is processed, and is convenient to promote in commercial Application.
The specific embodiment
Below with reference to the invention will be further described in conjunction with the embodiments.But the invention is not restricted to given example.
Embodiment 1
Taking 3.5g cerous nitrate, 2.5g aluminum nitrate and 2.5g magnesium nitrate is dissolved in 100mL deionized water, then take 7g13X molecular sieve and add in mixed solution, filter after flooding at normal temperatures 6h, washing, by gained sample roasting 4h at 400 ℃, obtain adsorbent.
Micro-moisture removes experiment: 0.3g adsorbent roasting 4h at 400 ℃ is activated, and then using the high pure nitrogen of 5N is unstripped gas, and at normal temperature, pressure is under 0.3MPa, to carry out dynamically water suction experiment, uses moisture monitor measurement result.
Result: dehydration degree of depth 40ppb, gas treatment amount 18940L.
Embodiment 2
Taking 3.5g cerous nitrate, 2.5g aluminum nitrate and 2.5g barium nitrate is dissolved in 100mL deionized water, then take 7g13X molecular sieve and add in mixed solution, filter after flooding at normal temperatures 12h, washing, by gained sample roasting 4h at 400 ℃, obtain adsorbent.
Micro-moisture removes experiment: 0.3g adsorbent roasting 4h at 350 ℃ is activated, and then using high-purity ammonia of 5N is unstripped gas, and at normal temperature, pressure is under 0.3MPa, to carry out dynamically water suction experiment, uses moisture monitor measurement result.
Result: dehydration degree of depth 41ppb, gas treatment amount 19089L.
Embodiment 3
Taking 3.5g cerous nitrate, 2.5g aluminum nitrate and 2.5g calcium nitrate is dissolved in 100mL deionized water, then take 7g13X molecular sieve and add in mixed solution, filter after flooding at normal temperatures 12h, washing, by gained sample roasting 4h at 400 ℃, obtain adsorbent.
Micro-moisture removes experiment: 0.3g adsorbent roasting 6h at 400 ℃ is activated, and then using the high-purity argon gas of 5N is unstripped gas, and at normal temperature, pressure is under 0.3MPa, to carry out dynamically water suction experiment, uses moisture monitor measurement result.
Result: dehydration degree of depth 38ppb, gas treatment amount 20156L.
Embodiment 4
Taking 3.5g cerous nitrate, 2.5g aluminum nitrate and 2.5g strontium nitrate is dissolved in 100mL deionized water, then take 7g13X molecular sieve and add in mixed solution, filter after flooding at normal temperatures 24h, washing, by gained sample roasting 4h at 400 ℃, obtain adsorbent.
Micro-moisture removes experiment: 0.3g adsorbent roasting 6h at 400 ℃ is activated, and then using the high pure nitrogen of 5N is unstripped gas, and at normal temperature, pressure is under 0.3MPa, to carry out dynamically water suction experiment, uses moisture monitor measurement result.
Result: dehydration degree of depth 35ppb, gas treatment amount 21579L.
Embodiment 5
Taking 3.5g cerous nitrate, 2.5g aluminum nitrate and 2.5g magnesium nitrate is dissolved in 100mL deionized water, then take 7g13X molecular sieve and add in mixed solution, filter after flooding at normal temperatures 6h, washing, by gained sample roasting 4h at 400 ℃, obtain adsorbent.
Micro-moisture removes experiment: 0.3g adsorbent roasting 6h at 360 ℃ is activated, and then using the high-purity argon gas of 5N is unstripped gas, and at normal temperature, pressure is under 0.25MPa, to carry out dynamically water suction experiment, uses moisture monitor measurement result.
Result: dehydration degree of depth 39ppb, gas treatment amount 20096L.
Embodiment 6
Taking 3.5g cerous nitrate, 2.5g aluminum nitrate and 2.5g barium nitrate is dissolved in 100mL deionized water, then take 7g13X molecular sieve and add in mixed solution, filter after flooding at normal temperatures 12h, washing, by gained sample roasting 4h at 400 ℃, obtain adsorbent.
Micro-moisture removes experiment: 0.3g adsorbent roasting 4h at 360 ℃ is activated, and then using the high purity oxygen gas of 5N is unstripped gas, and at normal temperature, pressure is under 0.25MPa, to carry out dynamically water suction experiment, uses moisture monitor measurement result.
Result: dehydration degree of depth 37ppb, gas treatment amount 19683L.
Embodiment 7
Taking 3.5g cerous nitrate, 2.5g aluminum nitrate and 2.5g calcium nitrate is dissolved in 100mL deionized water, then take 7g13X molecular sieve and add in mixed solution, filter after flooding at normal temperatures 12h, washing, by gained sample roasting 4h at 400 ℃, obtain adsorbent.
Micro-moisture removes experiment: 0.3g adsorbent roasting 8h at 360 ℃ is activated, and then using high-purity ammonia of 5N is unstripped gas, and at normal temperature, pressure is under 0.3MPa, to carry out dynamically water suction experiment, uses moisture monitor measurement result.
Result: dehydration degree of depth 36ppb, gas treatment amount 20549L.
Embodiment 8
Taking 3.5g cerous nitrate, 2.5g aluminum nitrate and 2.5g strontium nitrate is dissolved in 100mL deionized water, then take 7g13X molecular sieve and add in mixed solution, filter after flooding at normal temperatures 24h, washing, by gained sample roasting 4h at 400 ℃, obtain adsorbent.
Micro-moisture removes experiment: 0.3g adsorbent roasting 4h at 380 ℃ is activated, and then using the high pure nitrogen of 5N is unstripped gas, and at normal temperature, pressure is under 0.2MPa, to carry out dynamically water suction experiment, uses moisture monitor measurement result.
Result: dehydration degree of depth 38ppb, gas treatment amount 19125L.
Embodiment 9
Taking 3.5g cerous nitrate, 2.5g aluminum nitrate and 2.5g magnesium nitrate is dissolved in 100mL deionized water, then take 7g13X molecular sieve and add in mixed solution, filter after flooding at normal temperatures 24h, washing, by gained sample roasting 4h at 400 ℃, obtain adsorbent.
Micro-moisture removes experiment: 0.3g adsorbent roasting 6h at 400 ℃ is activated, and then using the high-purity argon gas of 5N is unstripped gas, and at normal temperature, pressure is under 0.3MPa, to carry out dynamically water suction experiment, uses moisture monitor measurement result.
Result: dehydration degree of depth 38ppb, gas treatment amount 19994L.
Embodiment 10
Taking 3.5g cerous nitrate, 2.5g aluminum nitrate and 1.5g barium nitrate is dissolved in 100mL deionized water, then take 7g13X molecular sieve and add in mixed solution, filter after flooding at normal temperatures 12h, washing, by gained sample roasting 4h at 400 ℃, obtain adsorbent.
Micro-moisture removes experiment: 0.3g adsorbent roasting 4h at 400 ℃ is activated, and then using the high pure nitrogen of 5N is unstripped gas, and at normal temperature, pressure is under 0.3MPa, to carry out dynamically water suction experiment, uses moisture monitor measurement result.
Result: dehydration degree of depth 35ppb, gas treatment amount 21696L.
Embodiment 11
Taking 3.5g cerous nitrate, 2.5g aluminum nitrate and 2.5g calcium nitrate is dissolved in 100mL deionized water, then take 7g13X molecular sieve and add in mixed solution, filter after flooding at normal temperatures 12h, washing, by gained sample roasting 4h at 400 ℃, obtain adsorbent.
Micro-moisture removes experiment: 0.3g adsorbent roasting 7h at 400 ℃ is activated, and then using the high pure nitrogen of 5N is unstripped gas, and at normal temperature, pressure is under 0.3MPa, to carry out dynamically water suction experiment, uses moisture monitor measurement result.
Result: dehydration degree of depth 36ppb, gas treatment amount 19038L.
Embodiment 12
Taking 3.5g cerous nitrate, 2.5g aluminum nitrate and 2.5g strontium nitrate is dissolved in 100mL deionized water, then take 7g13X molecular sieve and add in mixed solution, filter after flooding at normal temperatures 6h, washing, by gained sample roasting 4h at 400 ℃, obtain adsorbent.
Micro-moisture removes experiment: 0.3g adsorbent roasting 4h at 400 ℃ is activated, and then using the high pure nitrogen of 5N is unstripped gas, and at normal temperature, pressure is under 0.2MPa, to carry out dynamically water suction experiment, uses moisture monitor measurement result.
Result: dehydration degree of depth 37ppb, gas treatment amount 20467L.
Embodiment 13
Taking 3.5g cerous nitrate, 2.5g aluminum nitrate and 2.5g magnesium nitrate is dissolved in 100mL deionized water, then take 7g4A molecular sieve and add in mixed solution, filter after flooding at normal temperatures 12h, washing, by gained sample roasting 4h at 400 ℃, obtain adsorbent.
Micro-moisture removes experiment: 0.3g adsorbent roasting 6h at 350 ℃ is activated, and then using high-purity ammonia of 5N is unstripped gas, and at normal temperature, pressure is under 0.3MPa, to carry out dynamically water suction experiment, uses moisture monitor measurement result.
Result: dehydration degree of depth 37ppb, gas treatment amount 14500L.
Embodiment 14
Take 3.5g cerous nitrate, 2.5g aluminum nitrate and 2.5g barium nitrate and be dissolved in 100mL deionized water, then take 7g4A molecular sieve and add in mixed solution, filter after flooding at normal temperatures 6h, washing, by gained sample roasting 4h at 400 ℃, obtains adsorbent.
Micro-moisture removes experiment: 0.3g adsorbent roasting 4h at 360 ℃ is activated, and then using the high purity oxygen gas of 5N is unstripped gas, and at normal temperature, pressure is under 0.25MPa, to carry out dynamically water suction experiment, uses moisture monitor measurement result.
Result: dehydration degree of depth 38ppb, gas treatment amount 15820L.
Embodiment 15
Taking 3.5g cerous nitrate, 2.5g aluminum nitrate and 2.5g calcium nitrate is dissolved in 100mL deionized water, then take 7g4A molecular sieve and add in mixed solution, filter after flooding at normal temperatures 12h, washing, by gained sample roasting 4h at 400 ℃, obtain adsorbent.
Micro-moisture removes experiment: 0.3g adsorbent roasting 4h at 400 ℃ is activated, and then using the high purity oxygen gas of 5N is unstripped gas, and at normal temperature, pressure is under 0.2MPa, to carry out dynamically water suction experiment, uses moisture monitor measurement result.
Result: dehydration degree of depth 39ppb, gas treatment amount 17622L.
Embodiment 16
Taking 3.5g cerous nitrate, 2.5g aluminum nitrate and 2.5g magnesium nitrate is dissolved in 100mL deionized water, then take 7g4A molecular sieve and add in mixed solution, filter after flooding at normal temperatures 24h, washing, by gained sample roasting 4h at 400 ℃, obtain adsorbent.
Micro-moisture removes experiment: 0.3g adsorbent roasting 5h at 400 ℃ is activated, and then using the high pure nitrogen of 5N is unstripped gas, and at normal temperature, pressure is under 0.2MPa, to carry out dynamically water suction experiment, uses moisture monitor measurement result.
Result: dehydration degree of depth 36ppb, gas treatment amount 17862L.
Embodiment 17
Take 3.5g cerous nitrate, 2.5g aluminum nitrate and 2.5g barium nitrate and be dissolved in 100mL deionized water, then take 7g4A molecular sieve and add in mixed solution, filter after flooding at normal temperatures 6h, washing, by gained sample roasting 4h at 400 ℃, obtains adsorbent.
Micro-moisture removes experiment: 0.3g adsorbent roasting 4h at 380 ℃ is activated, and then using the high-purity argon gas of 5N is unstripped gas, and at normal temperature, pressure is under 0.25MPa, to carry out dynamically water suction experiment, uses moisture monitor measurement result.
Result: dehydration degree of depth 37ppb, gas treatment amount 16732L.
Embodiment 18
Taking 3.5g cerous nitrate, 2.5g aluminum nitrate and 2.5g calcium nitrate is dissolved in 100mL deionized water, then take 7g4A molecular sieve and add in mixed solution, filter after flooding at normal temperatures 12h, washing, by gained sample roasting 4h at 400 ℃, obtain adsorbent.
Micro-moisture removes experiment: 0.3g adsorbent roasting 4h at 390 ℃ is activated, and then using the high pure nitrogen of 5N is unstripped gas, and at normal temperature, pressure is under 0.3MPa, to carry out dynamically water suction experiment, uses moisture monitor measurement result.
Result: dehydration degree of depth 36ppb, gas treatment amount 16638L.
Embodiment 19
Taking 3.5g cerous nitrate, 2.5g aluminum nitrate and 2.5g strontium nitrate is dissolved in 100mL deionized water, then take 7g4A molecular sieve and add in mixed solution, filter after flooding at normal temperatures 24h, washing, by gained sample roasting 4h at 400 ℃, obtain adsorbent.
Micro-moisture removes experiment: 0.3g adsorbent roasting 4h at 395 ℃ is activated, and then using high-purity ammonia of 5N is unstripped gas, and at normal temperature, pressure is under 0.3MPa, to carry out dynamically water suction experiment, uses moisture monitor measurement result.
Result: dehydration degree of depth 38ppb, gas treatment amount 16593L.
Embodiment 20
Taking 3.5g cerous nitrate, 2.5g aluminum nitrate and 2.5g strontium nitrate is dissolved in 100mL deionized water, then take 7g4A molecular sieve and add in mixed solution, filter after flooding at normal temperatures 12h, washing, by gained sample roasting 4h at 400 ℃, obtain adsorbent.
Micro-moisture removes experiment: 0.3g adsorbent roasting 5h at 370 ℃ is activated, and then using high-purity ammonia of 5N is unstripped gas, and at normal temperature, pressure is under 0.25MPa, to carry out dynamically water suction experiment, uses moisture monitor measurement result.
Result: dehydration degree of depth 38ppb, gas treatment amount 16479L.
Comparative example
Use industrial widely used conventional dry drying prescription 13X and 4A molecular sieve to carry out micro-moisture and remove experiment, experimental technique is with embodiment 10.
13X molecular sieve experimental result: dehydration degree of depth 66ppb, gas treatment amount 4650L.
4A molecular sieve experimental result: dehydration degree of depth 51ppb, gas treatment amount 2602L.
Claims (9)
1. one kind for removing the adsorbent of gas micro-moisture, adsorbent described in it is characterized in that is that the method for the slaine modified molecular screen by being comprised of cerous nitrate, aluminum nitrate and other alkaline earth nitrate makes, the gross mass of molecular sieve after modification of take is benchmark, Ce elements mass percent is 0.02～10%, aluminium element mass percent is 0.05～3%, and other alkali earth metal mass percent is 0.08～10%.
2. according to claim 1 for removing the adsorbent of gas micro-moisture, it is characterized in that other described alkaline earth nitrate is one or more in magnesium nitrate, calcium nitrate, strontium nitrate and barium nitrate; Other described alkaline-earth metal is one or more in magnesium, calcium, strontium and barium.
3. according to claim 1 for removing the adsorbent of gas micro-moisture, it is characterized in that described molecular sieve is 13X molecular sieve or 4A molecular sieve.
One kind as described in as arbitrary in claim 1-3 for removing the preparation method of the adsorbent of gas micro-moisture, it is characterized in that comprising the following steps: cerous nitrate, aluminum nitrate and other alkaline earth nitrate are dissolved in and in deionized water, form solution, after adding molecular sieve dipping 6～24h under normal temperature, filter, washing, by the sample obtaining roasting 4～8h at 350～400 ℃, obtain for removing the adsorbent of gas micro-moisture.
5. according to claim 4 for removing the preparation method of the adsorbent of gas micro-moisture, it is characterized in that the concentration of described cerous nitrate in solution is 0.05～0.5mol/L, the concentration of aluminum nitrate in solution is 0.05～0.5mol/L, the concentration of other alkaline earth nitrate in solution is 0.05～0.5mol/L, and solution quality is 10～20 times of molecular sieve quality.
6. according to claim 4 for removing the preparation method of the adsorbent of gas micro-moisture, it is characterized in that other described alkaline earth nitrate is one or more in magnesium nitrate, calcium nitrate, strontium nitrate and barium nitrate.
7. according to claim 4 for removing the preparation method of the adsorbent of gas micro-moisture, it is characterized in that described molecular sieve is 13X molecular sieve or 4A molecular sieve.
One kind as described in as arbitrary in claim 1-3 for removing adsorbent application in micro-moisture in removing gas of gas micro-moisture.
9. according to claim 7 for removing adsorbent application in micro-moisture in removing gas of gas micro-moisture, it is characterized in that for removing high-purity N
2, high-purity O
2, high-purity H
2, high-purity N H
3, high-purity CH
4, high-purity C
2h
4or micro-moisture in rare gas.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107019999A (en) * | 2017-06-02 | 2017-08-08 | 福州大学 | The membrane separating method of micro-moisture in a kind of removing acetylene |
| CN108704453A (en) * | 2018-05-31 | 2018-10-26 | 佛山市高明区爪和新材料科技有限公司 | A kind of preparation method of air dewetting agent |
| CN109576029A (en) * | 2018-12-21 | 2019-04-05 | 大连海鑫化工有限公司 | A kind of desulfurizing dessicant and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1221775A (en) * | 1997-12-31 | 1999-07-07 | 中国科学院大连化学物理研究所 | Dewatering tech. for microwater in organic solvent |
| US20040168571A1 (en) * | 2001-04-02 | 2004-09-02 | Daniel Alvarez | Method for purification of lens gases used in photolithography |
| CN103396384A (en) * | 2013-08-06 | 2013-11-20 | 江苏阿尔法药业有限公司 | Adsorption process for removing low content water from tetrahydrofuran-methanol mixed solvent during production of statin drugs |
-
2014
- 2014-05-07 CN CN201410191434.4A patent/CN103933934B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1221775A (en) * | 1997-12-31 | 1999-07-07 | 中国科学院大连化学物理研究所 | Dewatering tech. for microwater in organic solvent |
| US20040168571A1 (en) * | 2001-04-02 | 2004-09-02 | Daniel Alvarez | Method for purification of lens gases used in photolithography |
| CN103396384A (en) * | 2013-08-06 | 2013-11-20 | 江苏阿尔法药业有限公司 | Adsorption process for removing low content water from tetrahydrofuran-methanol mixed solvent during production of statin drugs |
Non-Patent Citations (1)
| Title |
|---|
| 肖永厚等: "13X分子筛/氯化钙复合吸附剂用于净化乙烯中低浓度水分", 《天然气化工》, vol. 34, no. 3, 31 December 2009 (2009-12-31) * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107019999A (en) * | 2017-06-02 | 2017-08-08 | 福州大学 | The membrane separating method of micro-moisture in a kind of removing acetylene |
| CN108704453A (en) * | 2018-05-31 | 2018-10-26 | 佛山市高明区爪和新材料科技有限公司 | A kind of preparation method of air dewetting agent |
| CN109576029A (en) * | 2018-12-21 | 2019-04-05 | 大连海鑫化工有限公司 | A kind of desulfurizing dessicant and preparation method thereof |
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