CN107983296A - Insulated gas cylinder palladium oxide compound and preparation method - Google Patents
Insulated gas cylinder palladium oxide compound and preparation method Download PDFInfo
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- CN107983296A CN107983296A CN201711299707.7A CN201711299707A CN107983296A CN 107983296 A CN107983296 A CN 107983296A CN 201711299707 A CN201711299707 A CN 201711299707A CN 107983296 A CN107983296 A CN 107983296A
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- palladium oxide
- preparation
- oxide compound
- gas cylinder
- gelatinization
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C1/00—Pressure vessels, e.g. gas cylinder, gas tank, replaceable cartridge
- F17C1/12—Pressure vessels, e.g. gas cylinder, gas tank, replaceable cartridge with provision for thermal insulation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/25—Coated, impregnated or composite adsorbents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/10—Single element gases other than halogens
- B01D2257/108—Hydrogen
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/32—Hydrogen storage
Abstract
The invention discloses a kind of insulated gas cylinder palladium oxide compound and preparation method, which includes：1）Palladium oxide, cyclodextrin, water are subjected to gelatinization reaction so that gelatinization system is made；2）Nickel source, tin source, neodymia, dysprosia, butyl lithium, cetyl trimethylammonium bromide, hydrazine hydrate are added in gelatinization system to carry out hydro-thermal reaction, then filters, is dry with obtained solidfied material；3）By solidfied material ball milling with obtained insulated gas cylinder palladium oxide compound.The insulated gas cylinder can effectively inhale hydrogen with palladium oxide compound, while the preparation method has the advantages that process is simple and raw material is easy to get.
Description
Technical field
The present invention relates to insulated gas cylinder, and in particular, to a kind of insulated gas cylinder palladium oxide compound and preparation method.
Background technology
Insulated gas cylinder be it is existing industry or laboratory in a kind of common device, it is used for filling gas, as liquefied gas,
Helium, nitrogen, hydrogen etc..The most basic requirement of insulated gas cylinder is that to have excellent air-tightness and heat-insulating property, because containing
Or gas be harmful to for environment or human body, or be inflammable and explosive gas he, either which kind of gas he, once insulated gas cylinder
It will cause immeasurable loss and infringement for generation leakage.
At present, insulated gas cylinder is made of liner and overcoat.Either liner, overcoat itself, or liner and overcoat it
Between be to be assembled by welding procedure, and the weld seam formed in welding process be ensure insulated gas cylinder air-tightness extremely
Close important factor.Although constantly lifting welding procedure in the prior art, there are still insulated gas cylinder at present to use one
Air-tightness situation not up to standard after section.
The content of the invention
The object of the present invention is to provide a kind of insulated gas cylinder palladium oxide compound and preparation method, which uses
Palladium oxide compound can effectively inhale hydrogen, while the preparation method has the advantages that process is simple and raw material is easy to get.
To achieve these goals, the preparation method the present invention provides a kind of insulated gas cylinder with palladium oxide compound, bag
Include：
1）Palladium oxide, cyclodextrin, water are subjected to gelatinization reaction so that gelatinization system is made；
2）Nickel source, tin source, neodymia, dysprosia, butyl lithium, cetyl trimethylammonium bromide, hydrazine hydrate are added to gelatinization
To carry out hydro-thermal reaction in system, then filter, is dry with obtained solidfied material；
3）By solidfied material ball milling with obtained insulated gas cylinder palladium oxide compound.
Present invention also offers a kind of insulated gas cylinder palladium oxide compound, hot gas bottle palladium oxide compound passes through upper
The preparation method stated is prepared.
In the above-mentioned technical solutions, applicant of the present invention first by studying discovery for a long time：Insulated gas cylinder is being made
The reason for standby initial stage completed often possesses excellent air-tightness, but long-time is not up to standard using the air-tightness of rear insulated gas cylinder
It is to contain hydrogen in the gas in the cavity between liner and overcoat, and hydrogen is often right due to its molecular particle size is small
Weld seam causes to impact, so that weld seam constantly expands, so that insulated gas cylinder does not reach safety requirements.It is basic herein
On, the applicant inventor is prepared using palladium oxide as matrix by above-mentioned three-step approach, and with other metals or metal compound
Thing compound for composite, the compound can effectively absorb hydrogen.Thus, which can be positioned over
In cavity between liner and overcoat, to absorb hydrogen, so as to ensure that insulated gas cylinder has stable air-tightness.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Embodiment
The embodiment of the present invention is described in detail below.It is it should be appreciated that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to limit the invention.
A kind of preparation method the present invention provides insulated gas cylinder with palladium oxide compound, including：
1）Palladium oxide, cyclodextrin, water are subjected to gelatinization reaction so that gelatinization system is made；
2）Nickel source, tin source, neodymia, dysprosia, butyl lithium, cetyl trimethylammonium bromide, hydrazine hydrate are added to gelatinization
To carry out hydro-thermal reaction in system, then filter, is dry with obtained solidfied material；
3）By solidfied material ball milling with obtained insulated gas cylinder palladium oxide compound.
In the step 1 of the present invention）In, the dosage of each material can select in wide scope, but obtained in order to make
Palladium oxide compound has more excellent hydrogen-absorbing ability, it is preferable that in step 1）In, palladium oxide, cyclodextrin, the weight ratio of water are
10：4-7：20-30.
In the step 1 of the present invention）In, the dosage of each material can select in wide scope, but obtained in order to make
Palladium oxide compound has more excellent hydrogen-absorbing ability, it is preferable that in step 1）In, gelatinization reaction meets the following conditions：Reaction
Temperature is 50-65 DEG C, reaction time 4-6h.
In the step 1 of the present invention）In, the average grain diameter of palladium oxide can select in wide scope, but in order to make system
The palladium oxide compound obtained has more excellent hydrogen-absorbing ability, it is preferable that in step 1）In, the average grain diameter of palladium oxide is 30-
50nm。
In the step 2 of the present invention）In, the dosage of each material can select in wide scope, but obtained in order to make
Palladium oxide compound has more excellent hydrogen-absorbing ability, it is preferable that in step 2）In, gelatinization system, nickel source, tin source, neodymia,
Dysprosia, butyl lithium, cetyl trimethylammonium bromide, the weight ratio of hydrazine hydrate are 100：8-12：2-5：0.2-0.8：0.3-
0.6：0.05-0.15：2-4：11-16.
In the step 2 of the present invention）In, the condition of hydro-thermal reaction can select in wide scope, but in order to make to be made
Palladium oxide compound there is more excellent hydrogen-absorbing ability, it is preferable that preferably, in step 2）In, hydro-thermal reaction meets following
Condition：Carried out in closed environment, reaction temperature is 140-180 DEG C, reaction time 6-8h.
In the step 2 of the present invention）In, the specific species of nickel source can select in wide scope, but in order to make to be made
Palladium oxide compound there is more excellent hydrogen-absorbing ability, it is preferable that preferably, in step 2）In, nickel source for nickel acetate and/or
Nickel nitrate.
In the step 2 of the present invention）In, the specific species of tin source can select in wide scope, but in order to make to be made
Palladium oxide compound there is more excellent hydrogen-absorbing ability, it is preferable that preferably, tin source for butter of tin, tributyltin chloride
At least one of with triphenyl tin chloride.
In the step 2 of the present invention）In, dry condition can select in wide scope, but in order to make obtained oxygen
Changing palladium compound has more excellent hydrogen-absorbing ability, it is preferable that preferably, in step 2）In, drying meets the following conditions：It is dry
Temperature is 100-110 DEG C, drying time 2-3h.
In the step 3 of the present invention）In, the condition of ball milling can select in wide scope, but in order to make obtained oxygen
Changing palladium compound has more excellent hydrogen-absorbing ability, it is preferable that preferably, in step 3）In, the ball milling meets the following conditions：
The mass ratio of big ball and bead is 2：The mass ratio of 0.8-1.2, abrading-ball and material is 20：0.8-1.2, rotating speed 2000-
2200rpm, Ball-milling Time 25-35min.
Present invention also offers a kind of insulated gas cylinder palladium oxide compound, hot gas bottle palladium oxide compound passes through upper
The preparation method stated is prepared.
The present invention will be described in detail by way of examples below.
Embodiment 1
1）By palladium oxide（Average grain diameter is 40nm）, cyclodextrin, water is according to 10：5：25 weight ratio carries out gelatinization reaction（Reaction
Temperature is 55 DEG C, reaction time 5h）Gelatinization system is made；
2）By nickel source（Nickel acetate）, tin source（Butter of tin）, neodymia, dysprosia, butyl lithium, cetyl trimethyl bromination
Ammonium, hydrazine hydrate are added in gelatinization system to carry out hydro-thermal reaction（Carried out in closed environment, reaction temperature is 160 DEG C, instead
It is 7h between seasonable）, then filter, be dry（Drying temperature is 105 DEG C, drying time 2.5h）Solidfied material is made（It is gelatinized body
System, nickel source, tin source, neodymia, dysprosia, butyl lithium, cetyl trimethylammonium bromide, the weight ratio of hydrazine hydrate are 100：
10：3：0.5：0.4：0.09：3：13）；
3）By solidfied material ball milling（The mass ratio of big ball and bead is 2：1, the mass ratio of abrading-ball and material is 20：1, rotating speed is
2100rpm, Ball-milling Time 30min）Insulated gas cylinder palladium oxide compound A1 is made.
Embodiment 2
1）By palladium oxide（Average grain diameter is 30nm）, cyclodextrin, water is according to 10：4：20 weight ratio carries out gelatinization reaction（Reaction
Temperature is 50 DEG C, reaction time 4h）Gelatinization system is made；
2）By nickel source（Nickel nitrate）, tin source（Tributyltin chloride）, neodymia, dysprosia, butyl lithium, cetyl trimethyl bromine
Change ammonium, hydrazine hydrate is added in gelatinization system to carry out hydro-thermal reaction（Being carried out in closed environment, reaction temperature is 140 DEG C,
Reaction time is 6h）, then filter, be dry（Drying temperature is 100 DEG C, drying time 2h）Solidfied material is made（It is gelatinized body
System, nickel source, tin source, neodymia, dysprosia, butyl lithium, cetyl trimethylammonium bromide, the weight ratio of hydrazine hydrate are 100：8：
2：0.2：0.3：0.05：2：11）；
3）By solidfied material ball milling（The mass ratio of big ball and bead is 2：0.8, the mass ratio of abrading-ball and material is 20：0.8, rotating speed
For 2000rpm, Ball-milling Time 25min）Insulated gas cylinder palladium oxide compound A2 is made.
Embodiment 3
1）By palladium oxide（Average grain diameter is 50nm）, cyclodextrin, water is according to 10：7：30 weight ratio carries out gelatinization reaction（Reaction
Temperature is 65 DEG C, reaction time 6h）Gelatinization system is made；
2）By nickel source（Nickel nitrate）, tin source（Triphenyl tin chloride）, neodymia, dysprosia, butyl lithium, cetyl trimethyl bromine
Change ammonium, hydrazine hydrate is added in gelatinization system to carry out hydro-thermal reaction（Being carried out in closed environment, reaction temperature is 180 DEG C,
Reaction time is 8h）, then filter, be dry（Drying temperature is 110 DEG C, drying time 3h）Solidfied material is made（It is gelatinized body
System, nickel source, tin source, neodymia, dysprosia, butyl lithium, cetyl trimethylammonium bromide, the weight ratio of hydrazine hydrate are 100：
12：5：0.8：0.6：0.15：4：16）；
3）By solidfied material ball milling（The mass ratio of big ball and bead is 2：1.2, the mass ratio of abrading-ball and material is 20：1.2, rotating speed
For 2200rpm, Ball-milling Time 35min）Insulated gas cylinder palladium oxide compound A3 is made.
Comparative example 1
Method according to embodiment 1 carries out that palladium oxide compound B1 is made, the difference is that step 1）In be not used cyclodextrin.
Comparative example 2
Method according to embodiment 1 carries out that palladium oxide compound B2 is made, the difference is that step 2）In be not used nickel source.
Comparative example 3
Method according to embodiment 1 carries out that palladium oxide compound B3 is made, the difference is that step 2）In be not used tin source.
Comparative example 4
Method according to embodiment 1 carries out that palladium oxide compound B4 is made, the difference is that step 2）In be not used neodymia.
Comparative example 5
Method according to embodiment 1 carries out that palladium oxide compound B5 is made, the difference is that step 2）In be not used dysprosia.
Comparative example 6
Method according to embodiment 1 carries out that palladium oxide compound B6 is made, the difference is that step 2）In be not used butyl lithium.
Application examples 1
Above-mentioned palladium oxide compound A1-A3, B1-B6 are placed in the cavity between liner and overcoat so that adiabatic gas is made respectively
Bottle, while set and do not place palladium oxide compound in the cavity between contrast groups i.e. liner and overcoat；Then GB 24159- are passed through
2009 methods recorded carry out inflation/deflation to insulated gas cylinder until the air-tightness of insulated gas cylinder is undesirable, and finally statistics is adiabatic
The access times of gas cylinder, are specifically shown in Table 1.
Table 1
The preferred embodiment of the present invention described in detail above, still, the tool during present invention is not limited to the embodiments described above
Body details, in the range of the technology design of the present invention, can carry out a variety of simple variants, these letters to technical scheme
Monotropic type belongs to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should equally be considered as content disclosed in this invention.
Claims (10)
- A kind of 1. insulated gas cylinder preparation method of palladium oxide compound, it is characterised in that including：1）Palladium oxide, cyclodextrin, water are subjected to gelatinization reaction so that gelatinization system is made；2）By nickel source, tin source, neodymia, dysprosia, butyl lithium, cetyl trimethylammonium bromide, hydrazine hydrate described in To carry out hydro-thermal reaction in gelatinization system, then filter, is dry with obtained solidfied material；3）By the solidfied material ball milling with obtained insulated gas cylinder palladium oxide compound.
- 2. preparation method according to claim 1, wherein, in step 1）In, the palladium oxide, cyclodextrin, the weight of water Than for 10：4-7：20-30.
- 3. preparation method according to claim 1, wherein, in step 1）In, the gelatinization reaction meets the following conditions：Instead It is 50-65 DEG C to answer temperature, reaction time 4-6h.
- 4. preparation method according to claim 1, wherein, in step 1）In, the average grain diameter of the palladium oxide is 30- 50nm。
- 5. according to the preparation method described in any one in claim 1-4, wherein, in step 2）In, the gelatinization system, nickel Source, tin source, neodymia, dysprosia, butyl lithium, cetyl trimethylammonium bromide, the weight ratio of hydrazine hydrate are 100：8-12：2- 5：0.2-0.8：0.3-0.6：0.05-0.15：2-4：11-16.
- 6. preparation method according to claim 5, wherein, in step 2）In, the hydro-thermal reaction meets the following conditions： Carried out in closed environment, reaction temperature is 140-180 DEG C, reaction time 6-8h.
- 7. preparation method according to claim 5, wherein, in step 2）In, the nickel source is nickel acetate and/or nitric acid Nickel；Preferably, the tin source is at least one of butter of tin, tributyltin chloride and triphenyl tin chloride.
- 8. preparation method according to claim 5, wherein, in step 2）In, the drying meets the following conditions：Dry temperature Spend for 100-110 DEG C, drying time 2-3h.
- 9. the preparation method according to any one in claim 1-4,6-8, wherein, in step 3）In, the ball milling is expired Sufficient the following conditions：The mass ratio of big ball and bead is 2：The mass ratio of 0.8-1.2, abrading-ball and material is 20：0.8-1.2, rotating speed For 2000-2200rpm, Ball-milling Time 25-35min.
- 10. a kind of insulated gas cylinder palladium oxide compound, it is characterised in that the hot gas bottle palladium oxide compound passes through right It is required that the preparation method in 1-9 described in any one is prepared.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711299707.7A CN107983296A (en) | 2017-12-09 | 2017-12-09 | Insulated gas cylinder palladium oxide compound and preparation method |
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| CN201711299707.7A CN107983296A (en) | 2017-12-09 | 2017-12-09 | Insulated gas cylinder palladium oxide compound and preparation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115591533A (en) * | 2022-10-20 | 2023-01-13 | 兰州理工大学（Cn） | Graphene-based targeted hydrogen absorption nanocomposite and preparation method thereof |
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| CN115591533B (en) * | 2022-10-20 | 2023-09-05 | 兰州理工大学 | Graphene-based targeted hydrogen absorption nanocomposite and preparation method thereof |
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