CN107774098A - A kind of insulated gas cylinder molecular sieves compound material and preparation method - Google Patents
A kind of insulated gas cylinder molecular sieves compound material and preparation method Download PDFInfo
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- CN107774098A CN107774098A CN201711299712.8A CN201711299712A CN107774098A CN 107774098 A CN107774098 A CN 107774098A CN 201711299712 A CN201711299712 A CN 201711299712A CN 107774098 A CN107774098 A CN 107774098A
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- molecular sieves
- gas cylinder
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Classifications
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- 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
- B01D53/14—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 absorption
-
- 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
- B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
- B01D2252/40—Absorbents explicitly excluding the presence of water
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
- B01D2252/50—Combinations of absorbents
- B01D2252/504—Mixtures of two or more absorbents
-
- 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
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of insulated gas cylinder molecular sieves compound material and preparation method, the preparation method includes：1）Molecular sieve, hydrochloric acid, neopelex are subjected to priming reaction so that activation system is made；2）Magnesium source, palladium source, neodymia, dysprosia, butyl lithium, urea, sodium borohydride are added in activation system to carry out hydro-thermal reaction, then filters, dry so that solidfied material is made；3）By solidfied material ball milling with obtained insulated gas cylinder molecular sieves compound material.The insulated gas cylinder can effectively inhale hydrogen with molecular sieves compound material, while the preparation method has process simple and the advantages of raw material is easy to get.
Description
Technical field
The present invention relates to insulated gas cylinder, in particular it relates to a kind of insulated gas cylinder molecular sieves compound material and preparation side
Method.
Background technology
Insulated gas cylinder be it is existing industry or laboratory in commonly use a kind of 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
Generation leakage can then cause immeasurable loss and infringement.
At present, insulated gas cylinder is made up of inner bag and overcoat.Either inner bag, overcoat itself, or inner bag 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
It is an object of the invention to provide a kind of insulated gas cylinder molecular sieves compound material and preparation method, the insulated gas cylinder
Hydrogen can be effectively inhaled with molecular sieves compound material, while the preparation method has process simple and the advantages of raw material is easy to get.
To achieve these goals, the invention provides a kind of preparation method of insulated gas cylinder molecular sieves compound material,
Including：
1）Molecular sieve, hydrochloric acid, neopelex are subjected to priming reaction so that activation system is made；
2）Magnesium source, palladium source, neodymia, dysprosia, butyl lithium, urea, sodium borohydride are added in activation system to enter water-filling
Thermal response, then filter, dry so that solidfied material is made；
3）By solidfied material ball milling with obtained insulated gas cylinder molecular sieves compound material.
Present invention also offers a kind of insulated gas cylinder molecular sieves compound material, the hot gas bottle molecular sieves compound material leads to
Above-mentioned preparation method is crossed to be 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 inner bag and overcoat, and hydrogen is often right due to its molecular particle size is small
Weld seam impacts, and then weld seam is constantly expanded, and then causes insulated gas cylinder not reach safety requirements.It is basic herein
On, the applicant inventor is prepared using molecular sieve as matrix by above-mentioned three-step approach, and with other metals or metal compound
Thing carries out compound compound, and the compound can effectively absorb hydrogen.Thus, the molecular sieves compound material can be placed
In cavity between inner bag 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.
The invention provides a kind of preparation method of insulated gas cylinder molecular sieves compound material, including：
1）Molecular sieve, hydrochloric acid, neopelex are subjected to priming reaction so that activation system is made；
2）Magnesium source, palladium source, neodymia, dysprosia, butyl lithium, urea, sodium borohydride are added in activation system to enter water-filling
Thermal response, then filter, dry so that solidfied material is made；
3）By solidfied material ball milling with obtained insulated gas cylinder molecular sieves compound material.
In the step 1 of the present invention）In, the dosage of each material can select in wide scope, but in order that obtained
Molecular sieves compound material has more excellent hydrogen-absorbing ability, it is preferable that in step 1）In, molecular sieve, hydrochloric acid, detergent alkylate sulphur
The weight ratio of sour sodium is 10：2-3：0.2-0.5；Also, the pH of the hydrochloric acid is 5-6.5.
In the step 1 of the present invention）In, the dosage of each material can select in wide scope, but in order that obtained
Molecular sieves compound material has more excellent hydrogen-absorbing ability, it is preferable that in step 1）In, priming reaction meets following condition：Instead
It is 50-65 DEG C to answer temperature, reaction time 4-6h.
In the step 1 of the present invention）In, the average grain diameter of molecular sieve can select in wide scope, but in order that system
The molecular sieves compound material obtained has more excellent hydrogen-absorbing ability, it is preferable that in step 1）In, the average grain diameter of molecular sieve is
0.2-0.5mm。
In the step 2 of the present invention）In, the dosage of each material can select in wide scope, but in order that obtained
Molecular sieves compound material has more excellent hydrogen-absorbing ability, it is preferable that in step 2）In, activation system, magnesium source, palladium source, oxidation
Neodymium, dysprosia, butyl lithium, urea, the weight ratio of sodium borohydride are 100：15-22：4-6：0.1-0.5：0.3-0.6：0.1-
0.15：7-8：18-22.
In the step 2 of the present invention）In, the condition of hydro-thermal reaction can select in wide scope, but in order that be made
Molecular sieves compound material there is more excellent hydrogen-absorbing ability, it is preferable that preferably, in step 2）In, hydro-thermal reaction meet with
Lower condition：Carried out in closed environment, reaction temperature is 200-220 DEG C, reaction time 6-8h.
In the step 2 of the present invention）In, the specific species in magnesium source can select in wide scope, but in order that be made
Molecular sieves compound material there is more excellent hydrogen-absorbing ability, it is preferable that preferably, in step 2）In, magnesium source be magnesium acetate and/
Or magnesium nitrate.
In the step 2 of the present invention）In, the specific species in palladium source can select in wide scope, but in order that be made
Molecular sieves compound material there is more excellent hydrogen-absorbing ability, it is preferable that preferably, palladium source be palladium nitrate, palladium chloride, four
At least one of (triphenylphosphine) palladium.
In the step 2 of the present invention）In, dry condition can select in wide scope, but in order that obtained point
Son sieve composite has more excellent hydrogen-absorbing ability, it is preferable that preferably, in step 2）In, drying meets following condition：It is dry
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 that obtained point
Son sieve composite has more excellent hydrogen-absorbing ability, it is preferable that preferably, in step 3）In, the ball milling meets following bar
Part：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 molecular sieves compound material, the hot gas bottle molecular sieves compound material leads to
Above-mentioned preparation method is crossed to be prepared.
The present invention will be described in detail by way of examples below.
Embodiment 1
1）By molecular sieve（Average grain diameter is 0.3mm）, hydrochloric acid, neopelex is according to 10：2.5：0.4；It is also, described
The weight that the pH of hydrochloric acid is 5.5 is than carrying out priming reaction（Reaction temperature is 55 DEG C, reaction time 5h）So that activation system is made；
2）By magnesium source（Magnesium acetate）, palladium source（Palladium nitrate）, neodymia, dysprosia, butyl lithium, urea, sodium borohydride added to live
To carry out hydro-thermal reaction in change system（Carried out in closed environment, reaction temperature is 210 DEG C, reaction time 7h）, then
Filtering, dry（Drying temperature is 105 DEG C, drying time 2.5h）So that solidfied material is made（Activation system, magnesium source, palladium source, oxidation
Neodymium, dysprosia, butyl lithium, urea, the weight ratio of sodium borohydride are 100：20：5：0.3：0.4：0.12：7.5：20）；
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）So that insulated gas cylinder molecular sieves compound material A1 is made.
Embodiment 2
1）By molecular sieve（Average grain diameter is 0.2mm）, hydrochloric acid, neopelex is according to 10：2：0.2；Also, the salt
The weight that the pH of acid is 5 is than carrying out priming reaction（Reaction temperature is 50 DEG C, reaction time 4h）So that activation system is made；
2）By magnesium source（Magnesium nitrate）, palladium source（Palladium chloride）, neodymia, dysprosia, butyl lithium, urea, sodium borohydride be added to
To carry out hydro-thermal reaction in activation system（Carried out in closed environment, reaction temperature is 200 DEG C, reaction time 6h）, so
Filter, dry afterwards（Drying temperature is 100 DEG C, drying time 2h）So that solidfied material is made（Activation system, magnesium source, palladium source, oxidation
Neodymium, dysprosia, butyl lithium, urea, the weight ratio of sodium borohydride are 100：15：4：0.1：0.3：0.1：7：18）；
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）So that insulated gas cylinder molecular sieves compound material A2 is made.
Embodiment 3
1）By molecular sieve（Average grain diameter is 0.5mm）, hydrochloric acid, neopelex is according to 10： 3：0.5；It is also, described
The weight that the pH of hydrochloric acid is 6.5 is than carrying out priming reaction（Reaction temperature is 65 DEG C, reaction time 6h）So that activation system is made；
2）By magnesium source（Magnesium nitrate）, palladium source（Tetrakis triphenylphosphine palladium）, neodymia, dysprosia, butyl lithium, urea, sodium borohydride
Added in activation system to carry out hydro-thermal reaction（Carried out in closed environment, reaction temperature is 220 DEG C, and the reaction time is
8h）, then filter, dry（Drying temperature is 110 DEG C, drying time 3h）So that solidfied material is made（Activation system, magnesium source, palladium
Source, neodymia, dysprosia, butyl lithium, urea, the weight ratio of sodium borohydride are 100：22：6：0.5：0.6：0.15：8：22）；
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）So that insulated gas cylinder molecular sieves compound material A3 is made.
Comparative example 1
Method according to embodiment 1 carries out that molecular sieves compound material B1 is made, the difference is that step 1）In be not used hydrochloric acid.
Comparative example 2
Method according to embodiment 1 carries out that molecular sieves compound material B2 is made, the difference is that step 2）In be not used magnesium source.
Comparative example 3
Method according to embodiment 1 carries out that molecular sieves compound material B3 is made, the difference is that step 2）In be not used palladium source.
Comparative example 4
Method according to embodiment 1 carries out that molecular sieves compound material 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 molecular sieves compound material 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 molecular sieves compound material B6 is made, the difference is that step 2）In be not used butyl lithium.
Application examples 1
Above-mentioned molecular sieves compound material A1-A3, B1-B6 are placed in the cavity between inner bag and overcoat so that thermal insulation is made respectively
Gas cylinder, while set in the cavity between contrast groups i.e. inner bag and overcoat and do not place molecular sieves compound material；Then GB is passed through
24159-2009 record method to insulated gas cylinder carry out inflation/deflation until insulated gas cylinder air-tightness it is undesirable, finally unite
The access times of insulated gas cylinder are counted, are specifically shown in Table 1.
Table 1
The preferred embodiment of the present invention described in detail above, still, the present invention are not limited to the tool in above-mentioned embodiment
Body details, in the range of the technology design of the present invention, a variety of simple variants can be carried out to technical scheme, these letters
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. preparation method of insulated gas cylinder molecular sieves compound material, it is characterised in that including：1）Molecular sieve, hydrochloric acid, neopelex are subjected to priming reaction so that activation system is made；2）Magnesium source, palladium source, neodymia, dysprosia, butyl lithium, urea, sodium borohydride are added in the activation system to enter Water-filling thermal response, then filter, dry so that solidfied material is made；3）By the solidfied material ball milling with the obtained insulated gas cylinder molecular sieves compound material.
- 2. preparation method according to claim 1, wherein, in step 1）In, the molecular sieve, hydrochloric acid, detergent alkylate The weight ratio of sodium sulfonate is 10：2-3：0.2-0.5；Also, the pH of the hydrochloric acid is 5-6.5.
- 3. preparation method according to claim 1, wherein, in step 1）In, the priming reaction meets following condition：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 molecular sieve is 0.2- 0.5mm。
- 5. according to the preparation method described in any one in claim 1-4, wherein, in step 2）In, the activation system, magnesium Source, palladium source, neodymia, dysprosia, butyl lithium, urea, the weight ratio of sodium borohydride are 100：15-22：4-6：0.1-0.5： 0.3-0.6：0.1-0.15：7-8：18-22.
- 6. preparation method according to claim 5, wherein, in step 2）In, the hydro-thermal reaction meets following condition： Carried out in closed environment, reaction temperature is 200-220 DEG C, reaction time 6-8h.
- 7. preparation method according to claim 5, wherein, in step 2）In, the magnesium source is magnesium acetate and/or nitric acid Magnesium；Preferably, the palladium source is at least one of palladium nitrate, palladium chloride, tetrakis triphenylphosphine palladium.
- 8. preparation method according to claim 5, wherein, in step 2）In, the drying meets following condition：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 It is enough lower condition：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 molecular sieves compound material, it is characterised in that the hot gas bottle is passed through with molecular sieves compound material Preparation method in claim 1-9 described in any one is prepared.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711299712.8A CN107774098A (en) | 2017-12-09 | 2017-12-09 | A kind of insulated gas cylinder molecular sieves compound material and preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201711299712.8A CN107774098A (en) | 2017-12-09 | 2017-12-09 | A kind of insulated gas cylinder molecular sieves compound material and preparation method |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0395965A2 (en) * | 1989-05-05 | 1990-11-07 | Luz Industries Israel Ltd. | Device and method for removing gaseous impurities from a sealed vacuum |
| CN101658798A (en) * | 2008-08-29 | 2010-03-03 | 中国石油化工股份有限公司 | Method for modifying titanium silicate molecular sieve material |
| CN105570618A (en) * | 2015-12-10 | 2016-05-11 | 南京华东电子真空材料有限公司 | Combined type getter for improving hydrogen absorption performance |
| CN105715945A (en) * | 2016-03-14 | 2016-06-29 | 江苏德邦工程有限公司 | High-vacuum insulation low-temperature storage tank and manufacturing method thereof |
| CN107965661A (en) * | 2017-12-08 | 2018-04-27 | 芜湖市海格瑞德科技有限责任公司 | A kind of high stability liquefied natural gas mounted gas cylinder |
-
2017
- 2017-12-09 CN CN201711299712.8A patent/CN107774098A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0395965A2 (en) * | 1989-05-05 | 1990-11-07 | Luz Industries Israel Ltd. | Device and method for removing gaseous impurities from a sealed vacuum |
| CN101658798A (en) * | 2008-08-29 | 2010-03-03 | 中国石油化工股份有限公司 | Method for modifying titanium silicate molecular sieve material |
| CN105570618A (en) * | 2015-12-10 | 2016-05-11 | 南京华东电子真空材料有限公司 | Combined type getter for improving hydrogen absorption performance |
| CN105715945A (en) * | 2016-03-14 | 2016-06-29 | 江苏德邦工程有限公司 | High-vacuum insulation low-temperature storage tank and manufacturing method thereof |
| CN107965661A (en) * | 2017-12-08 | 2018-04-27 | 芜湖市海格瑞德科技有限责任公司 | A kind of high stability liquefied natural gas mounted gas cylinder |
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Application publication date: 20180309 |