WO2011010613A1 - Méthode d'alimentation en acétylène - Google Patents

Méthode d'alimentation en acétylène Download PDF

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Publication number
WO2011010613A1
WO2011010613A1 PCT/JP2010/062080 JP2010062080W WO2011010613A1 WO 2011010613 A1 WO2011010613 A1 WO 2011010613A1 JP 2010062080 W JP2010062080 W JP 2010062080W WO 2011010613 A1 WO2011010613 A1 WO 2011010613A1
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WO
WIPO (PCT)
Prior art keywords
acetylene
gas
moisture
hydride
purity
Prior art date
Application number
PCT/JP2010/062080
Other languages
English (en)
Japanese (ja)
Inventor
隆一郎 伊崎
Original Assignee
大陽日酸株式会社
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 大陽日酸株式会社 filed Critical 大陽日酸株式会社
Publication of WO2011010613A1 publication Critical patent/WO2011010613A1/fr

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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10HPRODUCTION OF ACETYLENE BY WET METHODS
    • C10H11/00Acetylene gas generators with submersion of the carbide in water
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00Purification; Separation; Use of additives
    • C07C7/12Purification; Separation; Use of additives by adsorption, i.e. purification or separation of hydrocarbons with the aid of solids, e.g. with ion-exchangers
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00Purification; Separation; Use of additives
    • C07C7/12Purification; Separation; Use of additives by adsorption, i.e. purification or separation of hydrocarbons with the aid of solids, e.g. with ion-exchangers
    • C07C7/13Purification; Separation; Use of additives by adsorption, i.e. purification or separation of hydrocarbons with the aid of solids, e.g. with ion-exchangers by molecular-sieve technique

Definitions

  • the present invention relates to a method for supplying acetylene, and more particularly to a method for supplying acetylene for supplying manufactured high-purity acetylene to a user.
  • Acetylene is used as a carbon source for these substances in processes for producing carbon nanotubes (CNT), carbon nanohorns (CNF), and silicon carbide (SiC) single crystals.
  • the acetylene used for this purpose is required to be highly pure with very few impurities.
  • various purification techniques and purification techniques have been conventionally used (see, for example, Patent Documents 1 to 4).
  • the method described in each patent document is mainly configured by a process of removing a solvent and a process of removing moisture.
  • a method is used in which degassing is carried out for a long time in the state of dissolved acetylene to remove impurities mainly composed of air components.
  • acetylene gas there is a problem that practicality is limited due to low gas purification efficiency and extremely high cost.
  • the amount of the high-purity acetylene gas obtained is extremely small, there is also a problem that it is difficult to supply to the use destination while maintaining high purity.
  • an object of the present invention is to provide a method for supplying acetylene, which can efficiently supply high-purity acetylene while maintaining a high-purity state at the use destination.
  • the moisture removal step of removing moisture contained in the gas by adsorbing it to the first dry adsorbent, and the gas after the moisture removal step being included in the gas by contacting the second dry adsorbent After obtaining high-purity acetylene by an acetylene production method comprising a hydride-removing step for removing hydride-based impurities, the obtained high-purity acetylene is supplied to the user at a pressure below atmospheric pressure
  • a method for supplying acetylene is provided.
  • the acetylene supply method of the present invention controls the amount of water supplied to the calcium carbide according to the amount of acetylene supplied to the acetylene use destination, and controls the acetylene gas generation step, water removal step, and hydride. It is characterized in that the inside of the system in the removal step is controlled to atmospheric pressure or lower.
  • the first dry adsorbent used in the water removal step is one of activated carbon and molecular sieves 3A or a mixture of activated carbon and molecular sieves 3A, and is used in the hydride removal step.
  • the second dry adsorbent is characterized by being one kind or a mixture of two or more kinds of activated alumina and molecular sieves 4A, 5A, 13X.
  • acetylene was obtained by a dry method that facilitates high purity, and impurities contained in the generated gas were separately purified and removed in the order of moisture and hydride impurities.
  • High purity acetylene can be efficiently supplied to the user.
  • high-purity acetylene can be supplied to the user more efficiently.
  • the present embodiment shows an example of an acetylene production and supply device for carrying out the acetylene supply method of the present invention, and includes a calcium carbide tank 11 filled with calcium carbide, and water is supplied to the calcium carbide tank 11.
  • a moisture supply device 12 that performs the adsorption and removal of moisture in the gas generated in the calcium carbide tank 11 by the first dry-type adsorbent, and a hydride in the gas by the second dry-type adsorbent.
  • Hydride removal purifier 14 for adsorbing and removing, acetylene supply line 15 for supplying purified high-purity acetylene to the consuming device used, first pressure gauge 16 for measuring the pressure of calcium carbide tank 11, and supply gas
  • the second pressure gauge 17 for measuring the pressure of the pressure and the surplus pressure discharge line 18 for discharging the surplus pressure are provided.
  • the procedure for supplying high-purity acetylene to the consumer using the acetylene production and supply apparatus having such a configuration will be described.
  • water liquid water or gaseous water vapor is supplied from the water supply device 12 to the calcium carbide tank 11, and the moisture is applied to the calcium carbide in the calcium carbide tank 11 to mainly contain acetylene.
  • An acetylene gas generation step for generating (crude acetylene gas) is performed.
  • the generated crude acetylene gas contains unreacted moisture and hydride impurities such as phosphine, hydrogen sulfide, and ammonia as reaction byproducts.
  • the crude acetylene gas derived from the calcium carbide tank 11 is introduced into the moisture removal purifier 13 to perform a moisture removal step.
  • a first dry adsorbent capable of removing moisture contained in the crude acetylene gas is used.
  • activated carbon or molecular sieves 3A which is an adsorbent that hardly adsorbs acetylene and can adsorb moisture, is optimal. You may use what filled only the activated carbon or only the molecular sieve 3A in the cylinder.
  • Activated carbon and molecular sieves 3A can be stacked and filled into the cylinder, or activated carbon and molecular sieves 3A can be mixed and filled into the cylinder.
  • the crude acetylene gas from which most of the contained water has been removed in the moisture removal step is introduced into the hydride removal purifier 14 and the hydride removal step is performed.
  • a second dry adsorbent that can remove hydride impurities such as phosphine, hydrogen sulfide, and ammonia contained in the crude acetylene gas is used.
  • the second dry adsorbent activated alumina, molecular sieves 4A, molecular sieves 5A, and molecular sieves 13X, which are adsorbents that hardly adsorb acetylene and can adsorb hydrides, are optimal.
  • a plurality of types can be filled in a cylinder and used.
  • the second dry adsorbent after removing moisture in the moisture removal step using the first dry adsorbent without simultaneously removing moisture and hydride, the second dry adsorbent was used.
  • the hydride is removed in the hydride removal step.
  • moisture content at the time of removing the hydride in crude acetylene gas is excluded, and adsorption removal of the hydride by a 2nd dry-type adsorption agent can be performed efficiently.
  • moisture and hydride can be simultaneously adsorbed and removed by using an appropriate adsorbent.
  • moisture and hydride are mixed, the hydride removal efficiency in the adsorbent decreases, and the hydride removal characteristics break through in a short time.
  • the treatment conditions of the moisture removal step are set so that the moisture concentration in the crude acetylene gas supplied from the moisture removal step to the hydride removal step is preferably 100 ppm or less, more preferably 10 ppm or less. Set. This makes it possible to reduce the concentration of hydrides other than acetylene to 0.1 ppm or less in the hydride removal step.
  • the high-purity acetylene which has been purified in high purity by removing moisture in the moisture removal step and hydride in the hydride removal step, is supplied to the consuming device through the acetylene supply line 15.
  • High-purity acetylene is supplied to the consuming device at a pressure below the atmospheric pressure in a state where it is sucked directly or indirectly through another device by a suction means such as a fan or a pump provided in the consuming device. It is consumed as a raw material for synthesizing nanomaterials (CNT, CNF) or as a carbon source in SiC semiconductor epitaxial growth.
  • the generation state of the crude acetylene gas and the supply state of the high purity acetylene are detected and controlled by the first pressure gauge 16 and the second pressure gauge 17. That is, when the measurement pressure of the first pressure gauge 16 decreases, the amount of moisture supplied from the moisture supply device 12 to the calcium carbide tank 11 is increased, and the amount of generation of crude acetylene gas is increased. When the measurement pressure of the first pressure gauge 16 rises, the amount of moisture supplied to the calcium carbide tank 11 is reduced to reduce the amount of generated crude acetylene gas. Further, when the measurement pressure of the second pressure gauge 17 decreases, the amount of water supplied from the water supply device 12 to the calcium carbide tank 11 is increased. When the measurement pressure of the second pressure gauge 17 rises, excess high-purity acetylene is extracted from the excess pressure release line 18 to keep the inside of the system below atmospheric pressure.
  • the amount of water supplied to the calcium carbide tank 11 is increased or decreased based on the measured pressures of the first pressure gauge 16 and the second pressure gauge 17, or surplus high-purity acetylene is removed from the surplus pressure release line 18 to the outside of the system.
  • the amount of acetylene generated can be accurately controlled.
  • the inside of the system of the acetylene production and supply apparatus including the acetylene supply line 15 can be maintained at a pressure below atmospheric pressure, and the high-purity acetylene is prevented from deteriorating and the desired amount of high-purity acetylene is efficiently supplied to the consumption apparatus Can be supplied.
  • the pressure in the system may be set according to the use state and acceptance state of the high-purity acetylene in the consuming device, and it is usually set to atmospheric pressure.
  • the method and means for causing moisture to act on the calcium carbide in the calcium carbide tank 11 are selected according to the size and shape of the calcium carbide tank 11, the amount and shape of calcium carbide in the tank, the amount of generation of crude acetylene gas, etc. can do.
  • liquid water can be supplied from the water supply device 12 to the calcium carbide tank 11 and dropped onto the calcium carbide.
  • the gaseous water vapor generated by the water supply device 12 can also be supplied to the calcium carbide tank 11. It is also possible to supply water in a gas-liquid mixed state into the calcium carbide tank 11.
  • the amount of water supplied to the calcium carbide tank 11 is preferably such that a large amount of water is not entrained in the crude acetylene gas, and as described above, the amount of moisture in the crude acetylene gas in the moisture removal step. It is desirable to set so that it can be easily reduced to 100 ppm or less.
  • the acetylene supplied by the acetylene supply method of the present invention is generated by a dry method that facilitates high purity, and impurities contained in the generated gas are separately purified and removed in the order of moisture and hydride impurities. high.
  • the high-purity acetylene gas can be easily handled because the high-purity acetylene is supplied to the user with the low-pressure gas. Therefore, the high purity acetylene can be efficiently supplied to the user by implementing the present invention near the user who consumes the high purity acetylene.
  • SYMBOLS 11 Calcium carbide tank, 12 ... Water supply apparatus, 13 ... Water removal refiner, 14 ... Hydride removal purifier, 15 ... Acetylene supply line, 16 ... First pressure gauge, 17 ... second pressure gauge, 18 ... excess pressure release line

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Drying Of Gases (AREA)

Abstract

La présente invention a pour objet une méthode d'alimentation en acétylène ayant pour objectif de fournir efficacement de l'acétylène de pureté élevée à un utilisateur. La méthode est caractérisée par la fourniture d'acétylène de pureté élevée à une pression allant jusqu'à la pression atmosphérique à un utilisateur d'acétylène, ledit acétylène de pureté élevée étant produit par un procédé qui comprend : une étape de production d'acétylène gaz consistant à faire réagir du carbure de calcium avec de l'eau pour produire un gaz contenant de l'acétylène en tant que composant principal ; une étape d'élimination de l'eau consistant à éliminer l'eau du gaz produit dans l'étape de production d'acétylène gaz en mettant le gaz en contact avec un premier adsorbant sec, provoquant de cette manière l'adsorption de l'eau contenue dans le gaz sur le premier adsorbant sec ; et une étape d'élimination des hydrures consistant à mettre le gaz qui a subi l'étape d'élimination de l'eau en contact avec un second adsorbant sec pour éliminer les impuretés de type hydrure contenues dans le gaz.
PCT/JP2010/062080 2009-07-21 2010-07-16 Méthode d'alimentation en acétylène WO2011010613A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2009170101A JP5583932B2 (ja) 2009-07-21 2009-07-21 アセチレンの製造方法
JP2009-170101 2009-07-21

Publications (1)

Publication Number Publication Date
WO2011010613A1 true WO2011010613A1 (fr) 2011-01-27

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JP (1) JP5583932B2 (fr)
TW (1) TWI495500B (fr)
WO (1) WO2011010613A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103130369A (zh) * 2011-12-05 2013-06-05 天辰化工有限公司 乙炔清净产生的次氯酸钠废水回用的一种方法
CN105969424A (zh) * 2016-07-07 2016-09-28 中盐吉兰泰盐化集团有限公司 一种利用回收电石灰尘生产乙炔气的系统

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102360179A (zh) * 2011-07-21 2012-02-22 新疆天业(集团)有限公司 干法乙炔生产中进出物料的控制方法
CN113731167B (zh) * 2021-09-02 2023-03-21 昆明理工大学 一种改性电石渣的制备方法及其产品和应用

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6245543A (ja) * 1985-08-22 1987-02-27 Toyo Soda Mfg Co Ltd 高純度アセチレンガスの製造法
JPH02256626A (ja) * 1988-08-25 1990-10-17 Taiyo Sanso Co Ltd 高純度アセチレンガスの製造方法
JP2004148257A (ja) * 2002-10-31 2004-05-27 Nichigo Acetylene Kk 可搬式超高純度アセチレン供給装置

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5768828A (en) * 1980-10-17 1982-04-27 Fuji Photo Film Co Ltd Diffusion transfer photography film unit

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6245543A (ja) * 1985-08-22 1987-02-27 Toyo Soda Mfg Co Ltd 高純度アセチレンガスの製造法
JPH02256626A (ja) * 1988-08-25 1990-10-17 Taiyo Sanso Co Ltd 高純度アセチレンガスの製造方法
JP2004148257A (ja) * 2002-10-31 2004-05-27 Nichigo Acetylene Kk 可搬式超高純度アセチレン供給装置

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103130369A (zh) * 2011-12-05 2013-06-05 天辰化工有限公司 乙炔清净产生的次氯酸钠废水回用的一种方法
CN103130369B (zh) * 2011-12-05 2014-07-02 天辰化工有限公司 乙炔清净产生的次氯酸钠废水回用的一种方法
CN105969424A (zh) * 2016-07-07 2016-09-28 中盐吉兰泰盐化集团有限公司 一种利用回收电石灰尘生产乙炔气的系统

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TWI495500B (zh) 2015-08-11
JP5583932B2 (ja) 2014-09-03
TW201111028A (en) 2011-04-01
JP2011026205A (ja) 2011-02-10

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