CN103349975B - The activation method of 5A molecular sieve - Google Patents
The activation method of 5A molecular sieve Download PDFInfo
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- CN103349975B CN103349975B CN201310329276.XA CN201310329276A CN103349975B CN 103349975 B CN103349975 B CN 103349975B CN 201310329276 A CN201310329276 A CN 201310329276A CN 103349975 B CN103349975 B CN 103349975B
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Abstract
The invention discloses a kind of activation method of 5A molecular sieve, comprise the following steps: 1) 5A molecular sieve is put into clean without after the container of greasy dirt, put into activation furnace heat-activated together with container, control activation temperature at 300 ~ 360 DEG C, control soak time 5 ~ 7 hours; 2) to come out of the stove air cooling after cooling to the 5A molecular sieve after activation with the furnace 140 ~ 160 DEG C; 3) cooled 5A molecular sieve is placed in the sealing of dried nitrogen atmosphere to deposit.The present invention strictly controls activation process, optimize activation temperature, improve the activation efficiency of commercially available 5A molecular sieve, and then significantly add the adsorption capacity of 5A molecular sieve, make it meet requirement as cryogenic insulated cylinder adsorbent, thus improve the thermal insulation of cryogenic insulated cylinder; Excellent with the 5A molecular sieve performance after the inventive method activation, water absorption rate is high, and absorption property is stablized, and molecular sieve is not easily pulverized, and is realizing, under the prerequisite that 5A molecular sieve fully activates, reducing energy consumption.
Description
Technical field
The present invention relates to the activation method of molecular sieve, refer to a kind of activation method of 5A molecular sieve particularly.
Background technology
The gas that material slowly can be released its absorption under vacuum conditions or be absorbed, in cryogenic insulated cylinder, the hydrogen etc. that material is released can reduce the vacuum of vacuum interlayer and cause the increase of heat output, therefore, in the vacuum interlayer of high vacuum cryogenic insulated cylinder, normal 5A molecular sieve and the palladium oxide of adopting is as adsorbent, wherein, generate water after the hydrogen that palladium oxide sorbing material is released, 5A molecular sieve is used for absorbing moisture.At present, commercially available 5A molecular sieve generally could normally need use through activation process, conventional activation method continues 8 hours or is heated to 550 DEG C continue 4 hours for 5A molecular sieve being heated to 250 DEG C, known after testing, 10% is no more than with the water absorption rate of the molecular sieve after front a kind of method activation, activate insufficient, and the water absorption rate of molecular sieve after adopting after the activation of a kind of method also only reaches 14% and 5A molecular sieve after activation is frangible, activation effect directly affects the realization of 5A molecular sieve function.Therefore, a kind of method finding out energy effective activation 5A molecular sieve is just very necessary.
Summary of the invention
Object of the present invention is exactly the activation method that will provide a kind of 5A molecular sieve, and the method can improve the water absorption rate of 5A molecular sieve, makes 5A molecular sieve fully can realize adsorption function, meets the requirement of cryogenic insulated cylinder adsorbent.
For achieving the above object, the technical solution used in the present invention is: a kind of activation method of 5A molecular sieve, and the method comprises the following steps:
1) 5A molecular sieve is put into totally without after the container of greasy dirt, put into activation furnace heat-activated together with container, control activation temperature at 300 ~ 360 DEG C, control soak time 5 ~ 7 hours;
2) to come out of the stove air cooling after cooling to the 5A molecular sieve after activation with the furnace 140 ~ 160 DEG C;
3) cooled 5A molecular sieve is placed in the sealing of dried nitrogen atmosphere to deposit, is adsorbed again into 5A molecular sieve to prevent the steam in air.
Further, in described step 1), controlling soak time is 345 ~ 355 DEG C, and controlling soak time is 5.5 ~ 6.5 hours.
Further, described step 2) in, air cooling of coming out of the stove after cooling to the 5A molecular sieve after activation with the furnace 145 ~ 155 DEG C.
Preferably, in described step 1), activation furnace is Muffle furnace.
Compared with prior art, tool of the present invention has the following advantages:
One, the present invention strictly controls activation process, optimize activation temperature, avoid the too low adsorbance affecting molecular sieve of temperature in prior art, and the too high saboteur of temperature sieves the phenomenon of crystal structure, improve the activation efficiency of commercially available 5A molecular sieve, and then significantly add the adsorption capacity of 5A molecular sieve, make it meet requirement as cryogenic insulated cylinder adsorbent, thus improve the thermal insulation of cryogenic insulated cylinder.
Its two, excellent with the 5A molecular sieve performance after the inventive method activation, water absorption rate is high, and absorption property is stablized, and molecular sieve is not easily pulverized, and is realizing, under the prerequisite that 5A molecular sieve fully activates, reducing energy consumption.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further illustrated, but the present invention is not limited to following embodiment.
Embodiment 1:
First, the airtight container acetone that 5A molecular sieve deposited by the frock container and sealing that are used for splendid attire 5A molecular sieve is cleaned up, to remove degreasing; Then, 10kg 5A molecular sieve is loaded in clean frock container, and put into activation furnace and carry out heat-activated, activation furnace is Muffle furnace, controlling activation in-furnace temperature is 350 DEG C, and soak time is 6 hours, air cooling of coming out of the stove after cooling to 150 DEG C after heat-activated completes with the furnace; Finally, with drying nitrogen, the 5A adsorbent of molecular sieve after activation process is left in clean airtight container by 1kg every part sealing.Wherein, nitrogen-sealed is the nitrogen after adopting liquid nitrogen gasification, carries out nitrogen displacement by cryogenic nitrogen gas cylinder vaporizer outlets access airtight container.
After tested, the water absorption rate of the 5A molecular sieve after this activation is 19.5%.
Embodiment 2
First, the airtight container acetone that 5A molecular sieve deposited by the frock container and sealing that are used for splendid attire 5A molecular sieve is cleaned up, to remove degreasing; Then, loaded in clean frock container by 10kg 5A molecular sieve, and put into activation furnace and carry out heat-activated, controlling activation in-furnace temperature is 300 DEG C, and soak time is 7 hours, air cooling of coming out of the stove after cooling to 140 DEG C after heat-activated completes with the furnace; Finally, with drying nitrogen, the 5A adsorbent of molecular sieve after activation process is left in clean airtight container by 1kg every part sealing.
After tested, the water absorption rate of the 5A molecular sieve after this activation is 19.0%.
Embodiment 3
First, the airtight container acetone that 5A molecular sieve deposited by the frock container and sealing that are used for splendid attire 5A molecular sieve is cleaned up, to remove degreasing; Then, loaded in clean frock container by 10kg 5A molecular sieve, and put into activation furnace and carry out heat-activated, controlling activation in-furnace temperature is 360 DEG C, and soak time is 5.5 hours, air cooling of coming out of the stove after cooling to 160 DEG C after heat-activated completes with the furnace; Finally, with drying nitrogen, the 5A adsorbent of molecular sieve after activation process is left in clean airtight container by 1kg every part sealing.
After tested, the water absorption rate of the 5A molecular sieve after this activation is 19.3%.
Embodiment 4
First, the airtight container acetone that 5A molecular sieve deposited by the frock container and sealing that are used for splendid attire 5A molecular sieve is cleaned up, to remove degreasing; Then, loaded in clean frock container by 10kg 5A molecular sieve, and put into activation furnace and carry out heat-activated, controlling activation in-furnace temperature is 345 DEG C, and soak time is 6.5 hours, air cooling of coming out of the stove after cooling to 155 DEG C after heat-activated completes with the furnace; Finally, with drying nitrogen, the 5A adsorbent of molecular sieve after activation process is left in clean airtight container by 1kg every part sealing.
After tested, the water absorption rate of the 5A molecular sieve after this activation is 20.3%.
Embodiment 5
First, the airtight container acetone that 5A molecular sieve deposited by the frock container and sealing that are used for splendid attire 5A molecular sieve is cleaned up, to remove degreasing; Then, loaded in clean frock container by 10kg 5A molecular sieve, and put into activation furnace and carry out heat-activated, controlling activation in-furnace temperature is 355 DEG C, and soak time is 5 hours, air cooling of coming out of the stove after cooling to 145 DEG C after heat-activated completes with the furnace; Finally, with drying nitrogen, the 5A adsorbent of molecular sieve after activation process is left in clean airtight container by 1kg every part sealing.
After tested, the water absorption rate of the 5A molecular sieve after this activation is 19.6%.
Claims (3)
1., for a 5A molecular sieve activation method for Cryo Heat Insulation absorption bottle adsorbent, it is characterized in that: the method comprises the following steps:
1) 5A molecular sieve is put into totally without after the container of greasy dirt, put into activation furnace heat-activated together with container, control activation temperature at 355 ~ 360 DEG C, control soak time 5.5 ~ 6.5 hours;
2) to come out of the stove air cooling after cooling to the 5A molecular sieve after activation with the furnace 140 ~ 160 DEG C;
3) cooled 5A molecular sieve is placed in the sealing of dried nitrogen atmosphere to deposit, is adsorbed again into 5A molecular sieve to prevent the steam in air.
2., according to claim 1 for the 5A molecular sieve activation method of Cryo Heat Insulation absorption bottle adsorbent, it is characterized in that: described step 2) in, air cooling of coming out of the stove after cooling to the 5A molecular sieve after activation with the furnace 145 ~ 155 DEG C.
3. according to claim 1 or 2, adsorb the 5A molecular sieve activation method of bottle adsorbent for Cryo Heat Insulation, it is characterized in that: described step 1) in, activation furnace is Muffle furnace.
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| US5914455A (en) * | 1997-09-30 | 1999-06-22 | The Boc Group, Inc. | Air purification process |
| CN103084141B (en) * | 2013-01-16 | 2015-06-03 | 昆明理工大学 | Modified 4a molecular sieve adsorbent and preparation method thereof |
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