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CN114057194A - A kind of method for preparing barium carbide and producing acetylene - Google Patents

A kind of method for preparing barium carbide and producing acetylene Download PDF

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Publication number
CN114057194A
CN114057194A CN202010777618.4A CN202010777618A CN114057194A CN 114057194 A CN114057194 A CN 114057194A CN 202010777618 A CN202010777618 A CN 202010777618A CN 114057194 A CN114057194 A CN 114057194A
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barium
carbide
acetylene
raw material
carbon
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CN114057194B (en
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姜标
赵虹
陈思远
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Shanghai Advanced Research Institute of CAS
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/90—Carbides
    • C01B32/914—Carbides of single elements
    • C01B32/935—Carbides of alkali metals, strontium, barium or magnesium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/40—Carbon monoxide
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00—Compounds of calcium, strontium, or barium
    • C01F11/02—Oxides or hydroxides
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10H—PRODUCTION OF ACETYLENE BY WET METHODS
    • C10H21/00—Details of acetylene generators; Accessory equipment for, or features of, the wet production of acetylene

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

本发明公开了一种制备碳化钡和生产乙炔的方法。将碳原料和钡原料按比例混合制备成粉状物料；将处理好的混合物料置于高温炉中，在非氧气气氛中加热到1300‑1650℃反应0.5‑4小时，制得碳化钡产物，该产物中碳化钡质量百分含量不低于60％。进一步将制备的碳化钡送入乙炔发生器中与水进行反应即得到乙炔气体。本发明采用碳化钡替代碳化钙来制备乙炔，可以在更加温和的条件下制备出含量较高的碳化钡，后期不需要经历液相碳化物冷却、脱模、破碎等复杂程序直接与水发气生成乙炔。与电石乙炔工艺相比，碳化钡乙炔工艺反应条件温和，工艺过程简单，可降低能耗减少排放，实现节能、降耗环保生产乙炔的目的。The invention discloses a method for preparing barium carbide and producing acetylene. The carbon raw material and the barium raw material are mixed in proportion to prepare a powdery material; the treated mixed material is placed in a high-temperature furnace, heated to 1300-1650 ℃ in a non-oxygen atmosphere and reacted for 0.5-4 hours to obtain a barium carbide product, The mass percentage content of barium carbide in the product is not less than 60%. Further, the prepared barium carbide is sent into an acetylene generator to react with water to obtain acetylene gas. In the present invention, barium carbide is used to replace calcium carbide to prepare acetylene, and barium carbide with higher content can be prepared under milder conditions, and it does not need to undergo complex procedures such as liquid-phase carbide cooling, demoulding, and crushing in the later stage. Acetylene is produced. Compared with the calcium carbide acetylene process, the barium carbide acetylene process has mild reaction conditions and simple process, which can reduce energy consumption and reduce emissions, and achieve the purpose of energy saving, consumption reduction and environmental protection production of acetylene.

Description

Method for preparing barium carbide and producing acetylene
Technical Field
The invention relates to the technical field of preparation of barium carbide and acetylene, in particular to a method for preparing barium carbide and producing acetylene.
Background
Acetylene is an important chemical basic raw material, can be used for producing acetaldehyde, acetic acid, chloroethylene, tetrachloroethane, vinyl acetylene and other ether and ester products through addition or polymerization reaction, and is widely usedThe composite material is widely applied to the novel energy fields of solvents, plastics, rubber, coatings, pesticides, synthetic fibers, solar cells, semiconductor materials and the like, and is called as 'the mother of organic chemical engineering'. China is a plurality of countries with coal, lean oil and little gas, and acetylene is mainly prepared by reacting calcium carbide prepared from coal with water to generate gas. Because the reaction process of the calcium carbide and water is simple, the key technology and cost control of the coal-based acetylene mainly lie in the preparation of the calcium carbide from coal. Calcium carbide of the chemical formula CaC2The industrial production is formed by the reaction of calcium oxide and coke. Because the reaction thermodynamic equilibrium temperature of calcium carbide generated by calcium oxide and coke is above 1780 ℃, in order to enhance the reaction process and accelerate the reaction speed, the reaction usually needs to form a melting tank at a high temperature of 2000-2200 ℃, so that liquid calcium oxide and solid carbon react in the melting tank to generate liquid calcium carbide, the liquid calcium carbide flows out of the furnace bottom of the calcium carbide electric-arc furnace, and the solid calcium carbide is obtained after cooling. The solid calcium carbide is crushed and then reacts with water to prepare acetylene. The production process of the calcium carbide has high temperature and high energy consumption, the electricity consumption of 1t of standard calcium carbide (the mass fraction of calcium carbide is 80%) produced at present is up to 3250-3400 kw, and how to save energy and reduce consumption is a key problem which needs to be solved urgently by the acetylene calcium carbide industry. Although patents 201610020462.9 and 201711403738.2 propose techniques for microwave synthesis of calcium carbide, which can reduce the synthesis temperature of calcium carbide from above 2000 ℃ to about 1750 ℃, the problem of high energy consumption in acetylene production cannot be fundamentally reduced due to the limitation of thermodynamic conditions of calcium carbide synthesis reaction.
In 1900, british patent GB19000782A proposed that carbides of barium, strontium or calcium could be produced with the by-product of iron sulfide by mixing barium sulfide or strontium sulfide or a mixture of calcium sulfide and carbon with other metals or metal oxides of iron or iron oxide and heating in a high temperature arc furnace. These metal carbides react with water to produce acetylene. Taking barium sulfide as an example, the chemical reaction formula is: BaS +2C + Fe ═ BaC2+FeS，BaC2+2H2O＝Ba(OH)2+C2H2. However, this patent only proposes such a chemical reaction route, and there is no description about the chemical reaction conditions such as reaction temperature, reaction time, and reactant ratio, etc., which determine whether the chemical reaction can be smoothly performed.
Chinese patent 200810233478.3 proposes a method for preparing a barium carbide electrolyte bulk material for use in the field of electrical insulation. The specific route is as follows: pressing a mixture of graphite and a barium compound with the mass percentage of 3-15% into a biscuit with certain strength and shape in a steel die under the pressure of 50-150MPa, and then sending the biscuit into a vacuum furnace for high-temperature treatment for the first time. And performing ball milling, refining and purification on the treated material, performing secondary steel die pressing again at the pressure of 400-600MPa, and then sending the material into the high-temperature furnace again for secondary high-temperature sintering to obtain the barium carbide serving as the electrolyte material. Although the method can synthesize barium carbide, the preparation method has long process and very harsh synthesis conditions, and not only needs to use graphite with high cost as a carbon source, but also needs to be pressed at the temperature of 1200 ℃ and 1450 ℃ after high pressure-6-10-4Pa, and the preparation period exceeds more than 15 h. On the other hand, the consumption of graphite in the raw material proportion is seriously insufficient, the consumption of the barium source is greatly excessive, the content of the barium dicarboxide in the product is low, and the gas generation requirement for producing acetylene gas can not be completely met. Therefore, the method is not suitable for the production of thousands of tons/year of acetylene in aspects of product quality characteristics, production cost, process complexity, production efficiency and the like.
Disclosure of Invention
The invention aims to provide a method for preparing barium carbide and producing acetylene, and aims to solve the problem that in the prior art, coal-based acetylene calcium carbide is harsh in synthesis conditions and high in energy consumption.
The technical scheme adopted by the invention for realizing the purpose is as follows:
a method of preparing barium carbide, the method comprising the steps of:
step 1, mixing a carbon raw material and a barium raw material in proportion to prepare a powdery material;
and 2, placing the treated mixed material in a high-temperature furnace, heating to 1300-1650 ℃ in a non-oxygen atmosphere, and reacting for 0.5-4 hours to obtain a barium carbide product, wherein the mass percentage of barium carbide in the product is not lower than 60%.
As a preferred embodiment, the carbon feedstock is selected from one or more of coal, coke, semi coke, coconut shell carbon or coal based carbon; the barium raw material is selected from one or more of barium carbonate, barium oxide and barium hydroxide.
As a preferred embodiment, the powder material has a particle size of not more than 2% on a 20 mesh sieve.
As a preferred embodiment, the powdery material is directly used as a reaction raw material, or a spherical material with a particle size of not more than 5cm is prepared by adopting wet granulation as the reaction raw material.
In a preferred embodiment, when barium carbonate or barium hydroxide is used as the barium source in the mixture of the carbon raw material and the barium raw material, the molar ratio of carbon to barium is (4.2 to 3.8): 1; when barium oxide is used as the barium source, the molar ratio of carbon to barium is (3.2-2.8): 1.
as a preferred embodiment, the high temperature furnace is a closed heating furnace, an electric heating mode is adopted, and the reaction temperature is 1500-1600 ℃.
As a preferred embodiment, the high temperature furnace is a closed heating furnace, a microwave heating mode is adopted, and the reaction temperature is 1300-1500 ℃.
As a preferred embodiment, the non-oxygen atmosphere is an argon or hydrogen atmosphere.
As a preferred embodiment, the reaction pressure is normal pressure or negative pressure, and the pressure range thereof is 0.001 to 0.3 atm.
The invention also provides a method for producing acetylene, which comprises the following steps:
step 1, mixing a carbon raw material and a barium raw material in proportion to prepare a powdery material;
step 2, placing the treated mixed material in a high-temperature furnace, heating to 1300-1650 ℃ in a non-oxygen atmosphere, and reacting for 0.5-4 hours to obtain a barium carbide product, wherein the mass percentage content of barium carbide in the product is not lower than 60%;
and 3, feeding the prepared barium carbide product into an acetylene generator to react with water to obtain acetylene gas.
Compared with the prior art, the invention has the following beneficial effects:
1, the acetylene is prepared by replacing calcium carbide with barium carbide, the barium carbide with higher content can be prepared under milder conditions, and the acetylene is directly generated with water without complex procedures of liquid-phase carbide cooling, demoulding, crushing and the like in the later period. Compared with the calcium carbide acetylene process, the barium carbide acetylene process has mild reaction conditions and simple process, can reduce energy consumption and emission, and achieves the purposes of energy conservation, consumption reduction and environmental protection for producing acetylene.
The invention provides a new industrial production path for preparing acetylene and co-producing carbon monoxide by synthesizing coal-based barium carbide under mild conditions, namely, a coal-based carbon source is adopted to react with barium compounds containing barium which can be decomposed into barium oxide, such as barium carbonate, barium oxide, barium hydroxide and other barium compounds which are not barium sulfide, barium carbide with the purity of over 80 percent is synthesized in a solid phase under mild conditions, and the barium carbide is further reacted with water to prepare acetylene. The whole process does not need high-pressure briquetting, and does not need to add other additives or catalysts such as iron oxide, copper oxide and the like and high vacuum conditions, and the reaction time is not more than 3 hours. Taking barium carbonate as an example, the principle is as follows: BaCO3+4C＝BaC2+3CO，BaC2+H2O＝Ba(OH)2+C2H2. In the whole process, only carbon monoxide and barium hydroxide are by-produced, wherein the carbon monoxide can be used as a raw material for processes such as MTO in C1 chemistry, and the barium hydroxide can be recycled and can also be separated and dried for other purposes. The barium carbide in the patent can be used for preparing acetylene gas, and can also be used in other fields such as electronics, materials and the like.
3, the invention discovers through experiments that: the energy consumption cost in the preparation process of the barium carbide and the acetylene can be further reduced by adopting a microwave heating mode. According to the data of the embodiment of the invention, the reaction temperature can be relatively lower and the reaction time is shorter by adopting a microwave heating mode compared with an electric heating mode.
4, the invention also finds out through experiments that: the product with higher barium carbide content can be obtained by introducing hydrogen or argon non-oxygen gas.
Detailed Description
The technical solution of the present invention will be described below with reference to specific examples. The starting materials and reagents used in the present invention are commercially available.
Example 1
The method comprises the following steps of (1) mixing blocky metallurgical coke (the fixed carbon content is 85%) and barium carbonate (the mass content of the barium carbonate is more than 98%) according to a carbon-barium molar ratio of 4: 1, processing the mixture into mixed powder with the granularity of more than 20 meshes and not more than 2 percent in a powder making machine after mixing, sending the mixed powder into a microwave heating furnace with an air extraction system, reacting for 60min at 1390-1420 ℃ and under the pressure of 0.01-0.02atm to obtain a product with the barium carbide mass percentage of 82-85 percent, sending the furnace gas into a CO purification process after heat exchange and dust removal, sending the barium carbide product into an acetylene generator after heat exchange to react with water to generate gas to obtain acetylene.
Example 2
Mixing semi-coke (the fixed carbon content is 87%) and barium carbonate (the mass content of barium carbonate is more than 98%) according to a carbon-barium molar ratio of 3.9: 1 are mixed and processed into mixed powder with the grain diameter of 40-80 meshes. The powder is sent into a microwave heating furnace with an air exhaust system and reacts for 60min at 1380-1410 ℃ and 0.015-0.02atm in hydrogen atmosphere to obtain a product with the barium carbide content of 89-93 percent by mass. And (3) after heat exchange and cooling, sending the barium carbide product into an acetylene generator to react with water to obtain acetylene, and sending furnace gas into a CO purification process after heat exchange and dust removal. As can be seen by comparing example 1 with example 2: the reaction in a hydrogen atmosphere can increase the content of barium carbide in the product.
Example 3
Coal-based activated carbon (with the fixed carbon content of 99%) and barium hydroxide (with the mass content of the barium hydroxide being more than 97%) are mixed according to the molar ratio of carbon to barium of 3.9: 1 is prepared into mixed powder with the granularity of 20-40 meshes. And (3) feeding the powder into an electric heating furnace, and reacting for 180min at 1520 ℃, 0.015-0.02atm and in an argon atmosphere to obtain a product with the barium carbide mass percentage of 86%. And (3) after heat exchange and cooling, sending the barium carbide product into an acetylene generator to react with water to obtain acetylene, and sending furnace gas into a CO purification process after heat exchange and dust removal.
Example 4
Anthracite (the fixed carbon content is 83 percent) and barium carbonate (the mass content of the barium carbonate is more than 98 percent) are mixed according to the mol ratio of the carbon to the barium of 4.2: 1, adding 25 percent of water for wet granulation to prepare small balls with the granularity of about 1 cm. Drying the pellets until the water content is less than 4%, sending the pellets into an electric heating furnace to react for 180min at 1570 ℃ under hydrogen atmosphere and 0.7-0.8atm to obtain a product with the barium carbide mass percentage of 60%, directly sending the generated barium carbide product into an acetylene generator to react with water to obtain acetylene gas, and sending the furnace gas into a CO purification process after heat exchange and dust removal.
Example 5
Mixing semi-coke (the fixed carbon content is 87%) and barium carbonate (the mass content of barium carbonate is more than 98%) according to a carbon-barium molar ratio of 3.9: 1, processing the mixture into mixed powder with the granularity of more than 30 meshes and not more than 1 percent, and adding 18 percent of water by mass ratio to perform wet granulation to obtain spherical materials with the grain diameter of 1 cm. Drying the formed spherical material until the water content is below 3%, heating the spherical material in an electric heating furnace to 1580 ℃ and reacting for 60min at 0.01-0.015tam to obtain a product with the barium carbide mass percentage of 88%. And directly feeding the generated barium carbide product into an acetylene generator to react with water to obtain acetylene gas, and feeding the furnace gas into a CO purification process after heat exchange and dust removal.
Example 6
Mixing semi-coke (the fixed carbon content is 87%) and barium oxide (the mass content of the barium oxide is more than 98%) according to a carbon-barium molar ratio of 3: 1 into mixed powder with the granularity of 80-120 meshes, sending the mixed powder into a microwave heating furnace, and reacting for 60min at 1450 ℃ and 0.001-0.005tam in argon atmosphere to obtain a product with the barium carbide content of 93 percent by mass. The generated barium carbide product is directly sent into an acetylene generator to react with water to obtain acetylene gas, and the furnace gas is sent into a CO purification process after heat exchange and dust removal.
The above description is only a part of the preferred embodiments of the present invention, and the present invention is not limited to the contents of the embodiments. It will be apparent to those skilled in the art that various changes and modifications can be made within the spirit of the invention, and any changes and modifications made are within the scope of the invention.

Claims (10)

1. A method of preparing barium carbide, the method comprising the steps of:
step 1, mixing a carbon raw material and a barium raw material in proportion to prepare a powdery material;
and 2, placing the treated mixed material in a high-temperature furnace, heating to 1300-1650 ℃ in a non-oxygen atmosphere, and reacting for 0.5-4 hours to obtain a barium carbide product, wherein the mass percentage of barium carbide in the product is not lower than 60%.
2. The method of producing barium carbide according to claim 1, wherein: the carbon raw material is selected from one or more of coal, coke, semi coke, coconut shell carbon or coal-based carbon; the barium raw material is selected from one or more of barium carbonate, barium oxide and barium hydroxide.
3. The method of producing barium carbide according to claim 1, wherein: the granularity of the powdery material is not more than 2 percent on a 20-mesh sieve.
4. The method of producing barium carbide according to claim 1, wherein: the powdery material is directly used as a reaction raw material, or a spherical material with the particle size of not more than 5cm is prepared by adopting wet granulation and is used as the reaction raw material.
5. The method of producing barium carbide according to claim 1, wherein: in the mixture of the carbon raw material and the barium raw material, when barium carbonate or barium hydroxide is used as a barium source, the molar ratio of carbon to barium is (4.2-3.8): 1; when barium oxide is used as the barium source, the molar ratio of carbon to barium is (3.2-2.8): 1.
6. the method of producing barium carbide according to claim 1, wherein: the high-temperature furnace is a closed heating furnace, an electric heating mode is adopted, and the reaction temperature is 1450-.
7. The method of producing barium carbide according to claim 1, wherein: the high-temperature furnace is a closed heating furnace, a microwave heating mode is adopted, and the reaction temperature is 1300-1500 ℃.
8. The method of producing barium carbide according to claim 1, wherein: the non-oxygen atmosphere is argon or hydrogen.
9. The method of producing barium carbide according to claim 1, wherein: the reaction pressure is normal pressure or negative pressure.
10. A process for producing acetylene, the process comprising the steps of:
step 1, mixing a carbon raw material and a barium raw material in proportion to prepare a powdery material;
step 2, placing the treated mixed material in a high-temperature furnace, heating to 1300-1650 ℃ in a non-oxygen atmosphere, and reacting for 0.5-4 hours to obtain a barium carbide product, wherein the mass percentage content of barium carbide in the product is not lower than 60%;
and 3, feeding the prepared barium carbide product into an acetylene generator to react with water to obtain acetylene gas.
CN202010777618.4A 2020-08-05 2020-08-05 Method for preparing barium carbide and producing acetylene Active CN114057194B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114538494A (en) * 2022-03-16 2022-05-27 中国科学院上海高等研究院 BaC2Recycling method of barium-based compound in acetylene preparation process

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB190007282A (en) * 1899-11-27 1901-03-16 Claude Marie Joseph Dit C Limb Improvements in or relating to the Production of Metallic Carbides and Derivatives therefrom.
FR682479A (en) * 1928-11-21 1930-05-28 Internat Ind & Chemical Compan Preparation of barium carbide and application to the continuous production of acetylene and barium hydrate
FR1304984A (en) * 1961-11-03 1962-09-28 Ionics Process for the preparation of metal carbides and acetylene, plant for carrying out the present process or similar process and products conforming to those obtained by the present process or similar process
CN101391769A (en) * 2008-10-24 2009-03-25 昆明理工大学 Preparation of Barium Carbon Dielectric Bulk Materials by Reactive Synthesis
CN106744844A (en) * 2016-12-23 2017-05-31 武汉理工大学 A kind of method by carrying out chlorination controlledly synthesis high-quality Graphene to two-dimentional carbide crystalline

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB190007282A (en) * 1899-11-27 1901-03-16 Claude Marie Joseph Dit C Limb Improvements in or relating to the Production of Metallic Carbides and Derivatives therefrom.
FR682479A (en) * 1928-11-21 1930-05-28 Internat Ind & Chemical Compan Preparation of barium carbide and application to the continuous production of acetylene and barium hydrate
FR1304984A (en) * 1961-11-03 1962-09-28 Ionics Process for the preparation of metal carbides and acetylene, plant for carrying out the present process or similar process and products conforming to those obtained by the present process or similar process
CN101391769A (en) * 2008-10-24 2009-03-25 昆明理工大学 Preparation of Barium Carbon Dielectric Bulk Materials by Reactive Synthesis
CN106744844A (en) * 2016-12-23 2017-05-31 武汉理工大学 A kind of method by carrying out chlorination controlledly synthesis high-quality Graphene to two-dimentional carbide crystalline

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114538494A (en) * 2022-03-16 2022-05-27 中国科学院上海高等研究院 BaC2Recycling method of barium-based compound in acetylene preparation process
CN114538494B (en) * 2022-03-16 2023-09-22 中国科学院上海高等研究院 A method for recycling barium-based compounds in the process of producing acetylene from BaC2

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