阅读说明：本技术 高纯硫化氢的制备工艺 (Preparation process of high-purity hydrogen sulfide ) 是由 曾令军 汪正宏 阳辉 曾令霞 于 2020-06-30 设计创作，主要内容包括：本发明提供了一种高纯硫化氢的制备工艺,包括：步骤S1、依次将硫磺、有机溶剂及1,2-双(二苯基膦)乙烷加入反应釜中,搅拌混匀,以第一加热温度加热至硫磺熔融成液态,得液态熔融物；步骤S2、往所述熔融物中通入氢气,反应、收集气体,得粗品硫化氢；步骤S3、将所述粗品硫化氢通入吸附装置,干燥,得低水分硫化氢；步骤S4、将低水分硫化氢通入粗品罐,收集第一时间,得收集硫化氢；步骤S5、将所述收集硫化氢通入一级成品罐,在第二温度和第二压力下脱除重组分杂质,得一级硫化氢；步骤S6、将所述一级硫化氢通入二级成品罐,在第三温度和第三压力下脱除轻组分杂质,得高纯硫化氢。解决了传统高纯硫化氢的制备工艺无法工业化生产的技术问题。(The invention provides a preparation process of high-purity hydrogen sulfide, which comprises the following steps: step S1, sequentially adding sulfur, an organic solvent and 1, 2-bis (diphenylphosphino) ethane into a reaction kettle, uniformly stirring, and heating at a first heating temperature until the sulfur is molten into a liquid state to obtain a liquid melt; step S2, introducing hydrogen into the melt, reacting, and collecting gas to obtain crude hydrogen sulfide; step S3, introducing the crude hydrogen sulfide into an adsorption device, and drying to obtain low-moisture hydrogen sulfide; step S4, introducing the low-moisture hydrogen sulfide into a crude product tank, and collecting for the first time to obtain collected hydrogen sulfide; step S5, introducing the collected hydrogen sulfide into a primary finished product tank, and removing heavy component impurities at a second temperature and a second pressure to obtain primary hydrogen sulfide; and step S6, introducing the primary hydrogen sulfide into a secondary finished product tank, and removing light component impurities at a third temperature and a third pressure to obtain high-purity hydrogen sulfide. Solves the technical problem that the traditional preparation process of high-purity hydrogen sulfide can not realize industrial production.)

1. A preparation process of high-purity hydrogen sulfide is characterized by comprising the following steps:

step S1, sequentially adding sulfur, an organic solvent and 1, 2-bis (diphenylphosphino) ethane into a reaction kettle, uniformly stirring, and heating at a first heating temperature until the sulfur is molten into a liquid state to obtain a liquid melt;

step S2, introducing hydrogen into the melt in the step S1, reacting, and collecting gas to obtain crude hydrogen sulfide;

step S3, introducing the crude hydrogen sulfide prepared in the step S2 into an adsorption device, and drying to obtain low-moisture hydrogen sulfide;

step S4, introducing the low-moisture hydrogen sulfide obtained in the step S3 into a crude product tank, and collecting for the first time to obtain collected hydrogen sulfide;

s5, introducing the collected hydrogen sulfide obtained in the step S4 into a primary finished product tank, and removing heavy component impurities at a second temperature and a second pressure to obtain primary hydrogen sulfide;

and S6, introducing the primary hydrogen sulfide obtained in the step S5 into a secondary finished product tank, and removing light component impurities at a third temperature and a third pressure to obtain high-purity hydrogen sulfide.

2. The process for producing high purity hydrogen sulfide according to claim 1, wherein in the step S1, the mass ratio of the sulfur to the 1, 2-bis (diphenylphosphino) ethane is 1000: (1-2); and/or the presence of a gas in the gas,

in step S1, the mass ratio of the sulfur to the organic solvent is 1: (5-8).

3. The process for preparing high-purity hydrogen sulfide according to claim 2, wherein in the step S1, the temperature in the reaction kettle is 40 to 60 ℃; and/or the presence of a gas in the gas,

in the step S1, the pressure of the reaction kettle is 0.05-0.15 MPa.

4. The process for producing highly pure hydrogen sulfide according to claim 3, wherein in step S1, the organic solvent is an aromatic compound.

5. The process for producing high-purity hydrogen sulfide according to claim 1, wherein in the step S2, the purity of the introduced hydrogen gas is 99.9% or more; and/or the presence of a gas in the gas,

in the step S2, the flow rate of the introduced hydrogen is 5-15 m³/h。

6. The process for producing high purity hydrogen sulfide according to claim 1, wherein in the step S3, the adsorbent is a 4A molecular sieve or a 5A molecular sieve; and/or the presence of a gas in the gas,

in the step S3, the adsorption temperature in the adsorption device is less than or equal to 40 ℃.

7. The process for producing highly pure hydrogen sulfide according to claim 1, wherein the first time period in step S4 is 1 to 3 hours.

8. The process for producing high purity hydrogen sulfide according to any one of claims 1 to 6, wherein the sulfur in step S1 is in the form of powder; and/or the presence of a gas in the gas,

the purity of the sulfur is greater than or equal to 95%.

9. The process for producing high-purity hydrogen sulfide according to any one of claims 1 to 6, wherein in the step S5, the second temperature is in the range of-30 ℃ to-20 ℃; and/or the presence of a gas in the gas,

the second pressure is-0.05 to-0.08 MPa.

10. The process for producing high-purity hydrogen sulfide according to any one of claims 1 to 6, wherein in the step S6, the third temperature is in the range of-55 ℃ to-45 ℃; and/or the presence of a gas in the gas,

the third pressure is-0.05 to-0.06 MPa.

Technical Field

The invention relates to the technical field of high-purity gas preparation, in particular to a preparation process of high-purity hydrogen sulfide.

Background

Hydrogen sulfide is an important chemical raw material, and is mainly used for synthesis of fine organic chemicals, inorganic salts and the like, such as production of pesticides and medicinal products, purification of metals, production of various industrial reagents and the like. In the related art, there are various methods for synthesizing hydrogen sulfide: the method is characterized in that liquid sulfur is dissolved in a solvent, and hydrogen is introduced into the solvent to prepare hydrogen sulfide gas, although the early reaction is good, the solvent generates a coking phenomenon along with the reaction, so that the reaction efficiency is reduced, and the industrial production is difficult to realize; secondly, the sulfur steam and the hydrogen are directly adopted to synthesize the hydrogen sulfide gas, although the method is simple to operate, the method has higher requirement on a reaction device, the temperature of the whole reaction is higher and is difficult to control, and the reaction heat can not be recycled, so that the conversion rate of the hydrogen sulfide gas is low, and the industrial production is difficult. Therefore, a preparation process of high-purity hydrogen sulfide suitable for industrial production is imperative.

Disclosure of Invention

Aiming at the defects in the prior art, the invention provides a preparation process of high-purity hydrogen sulfide, which aims to solve the technical problem that the traditional preparation of high-purity hydrogen sulfide in the related art can not realize industrial production.

The invention provides a preparation process of high-purity hydrogen sulfide, which comprises the following steps:

step S1, sequentially adding sulfur, an organic solvent and 1, 2-bis (diphenylphosphino) ethane into a reaction kettle, uniformly stirring, and heating at a first heating temperature until the sulfur is molten into a liquid state to obtain a liquid melt;

step S2, introducing hydrogen into the melt in the step S1, reacting, and collecting gas to obtain crude hydrogen sulfide;

step S3, introducing the crude hydrogen sulfide prepared in the step S2 into an adsorption device, and drying to obtain low-moisture hydrogen sulfide;

step S4, introducing the low-moisture hydrogen sulfide obtained in the step S3 into a crude product tank, and collecting for the first time to obtain collected hydrogen sulfide;

s5, introducing the collected hydrogen sulfide obtained in the step S4 into a primary finished product tank, and removing heavy component impurities at a second temperature and a second pressure to obtain primary hydrogen sulfide;

and S6, introducing the primary hydrogen sulfide obtained in the step S5 into a secondary finished product tank, and removing light component impurities at a third temperature and a third pressure to obtain high-purity hydrogen sulfide.

Alternatively, in the step S1, the mass ratio of the sulfur to the 1, 2-bis (diphenylphosphino) ethane is 1000: (1-2); and/or the presence of a gas in the gas,

in step S1, the mass ratio of the sulfur to the organic solvent is 1: (5-8).

Optionally, in the step S1, the temperature in the reaction kettle is 40-60 ℃; and/or the presence of a gas in the gas,

in the step S1, the pressure of the reaction kettle is 0.05-0.15 MPa.

Alternatively, in the step S1, the organic solvent is an aromatic compound.

Optionally, in the step S2, the purity of the introduced hydrogen is greater than or equal to 99.9%; and/or the presence of a gas in the gas,

in the step S2, the flow rate of the introduced hydrogen is 5-15 m³/h。

Alternatively, in the step S3, the adsorbent is 4A molecular sieve or 5A molecular sieve; and/or the presence of a gas in the gas,

in the step S3, the adsorption temperature in the adsorption device is less than or equal to 40 ℃.

Optionally, in the step S4, the first time is 1-3 h.

Optionally, the sulfur in step S1 is in powder form; and/or the presence of a gas in the gas,

the purity of the sulfur is greater than or equal to 95%.

Optionally, in the step S5, the second temperature is-30 to-20 ℃; and/or the presence of a gas in the gas,

the second pressure is-0.05 to-0.08 MPa.

Optionally, in the step S6, the third temperature is-55 to-45 ℃; and/or the presence of a gas in the gas,

the third pressure is-0.05 to-0.06 MPa.

Compared with the prior art, the invention has the following beneficial effects:

in the technology of the invention, a new process for synthesizing hydrogen sulfide by sulfur and hydrogen is provided, namely, the sulfur, an organic solvent and 1, 2-bis (diphenylphosphino) ethane are co-melted to form a co-melt; hydrogen sulfide gas is then produced by adding hydrogen to the eutectic. The whole process has the advantages of short implementation flow, compact equipment, high automatic control degree, large gas production, stable product gas quality, easy control and operation of the whole flow and convenient industrial production. In addition, the temperature of the whole process flow is lower, the exothermic energy in the reaction process is better controlled, and the conversion of hydrogen sulfide is increased.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more clearly apparent, the technical solutions of the present invention are further described below with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.

The invention provides a preparation process of high-purity hydrogen sulfide, which comprises the following steps:

step S1, sequentially adding sulfur, an organic solvent and 1, 2-bis (diphenylphosphino) ethane into a reaction kettle, uniformly stirring, and heating at a first heating temperature until the sulfur is molten into a liquid state to obtain a liquid melt;

step S2, introducing hydrogen into the melt in the step S1, reacting, and collecting gas to obtain crude hydrogen sulfide;

step S3, introducing the crude hydrogen sulfide prepared in the step S2 into an adsorption device, and drying to obtain low-moisture hydrogen sulfide;

step S4, introducing the low-moisture hydrogen sulfide obtained in the step S3 into a crude product tank, and collecting for the first time to obtain collected hydrogen sulfide;

s5, introducing the collected hydrogen sulfide obtained in the step S4 into a primary finished product tank, and removing heavy component impurities at a second temperature and a second pressure to obtain primary hydrogen sulfide;

and S6, introducing the primary hydrogen sulfide obtained in the step S5 into a secondary finished product tank, and removing light component impurities at a third temperature and a third pressure to obtain high-purity hydrogen sulfide.

In this embodiment, a new process for synthesizing hydrogen sulfide from sulfur and hydrogen is provided, in which sulfur, an organic solvent, and 1, 2-bis (diphenylphosphino) ethane are co-melted to form a co-melt; hydrogen sulfide gas is then produced by adding hydrogen to the eutectic. The whole process has the advantages of short implementation flow, compact equipment, high automatic control degree, large gas production, stable product gas quality, easy control and operation of the whole flow and convenient industrial production. In addition, the temperature of the whole process flow is lower, the exothermic energy in the reaction process is better controlled, and the conversion of hydrogen sulfide is increased.

Specifically, firstly, melting sulfur, an organic solvent and 1, 2-bis (diphenylphosphino) ethane together according to a certain proportion to form a eutectic; then introducing high-purity hydrogen into the lower part of the eutectic to realize the complete reaction of the liquid sulfur and the hydrogen and generate a crude hydrogen sulfide gas; then introducing the crude hydrogen sulfide gas from the lower part of an adsorption device, adsorbing and dehydrating by an adsorbent, and then discharging from the upper part of the adsorption device to obtain low-moisture hydrogen sulfide; introducing the low-moisture hydrogen sulfide gas into the upper part of a primary finished product tank to remove heavy component impurities (such as aromatic solvents, metal impurities and the like) in the low-moisture hydrogen sulfide gas through low-temperature and low-pressure condensation to obtain primary hydrogen sulfide coming out of the upper part of the primary finished product tank; finally, introducing the primary hydrogen sulfide gas into the upper part of a secondary finished product tank, removing light component impurities (such as nitrogen, hydrogen, methane, carbon dioxide and the like) in the primary hydrogen sulfide at low temperature and low pressure, and discharging the light component impurities from the upper part of the secondary finished product tank; the high-purity hydrogen sulfide is filled into the bottle through a filling pipe which is introduced into the bottom of the secondary finished product tank.

Alternatively, in the step S1, the mass ratio of the sulfur to the 1, 2-bis (diphenylphosphino) ethane is 1000: (1-2); and/or the presence of a gas in the gas,

in step S1, the mass ratio of the sulfur to the organic solvent is 1: (5-8).

In this embodiment, for example, but not limited to, the mass ratio of the sulfur to the 1, 2-bis (diphenylphosphino) ethane is 1: 1.5. for example, but not limited to, the mass ratio of the sulfur to the organic solvent is 1: 6.

Optionally, in the step S1, the temperature in the reaction kettle is 40-60 ℃; and/or the presence of a gas in the gas,

in the step S1, the pressure of the reaction kettle is 0.05-0.15 MPa.

In this embodiment, for example, but not limiting of, the temperature in the reaction kettle is 50 ℃. For example, but not limiting of, the pressure in the reaction kettle is 1.0 MPa.

Alternatively, in the step S1, the organic solvent is an aromatic compound.

In this embodiment, for example, but not limited to, the aromatic compound is one or a combination of m-xylene, o-xylene, and p-xylene.

Optionally, in the step S2, the purity of the introduced hydrogen is greater than or equal to 99.9%; and/or the presence of a gas in the gas,

in the step S2, the flow rate of the introduced hydrogen is 5-15 m³/h。

In this embodiment, for example, but not limited to, the purity of the introduced hydrogen gas is 99.99%. For example, but not limited to, the flow rate of the introduced hydrogen gas is 7.5m³/h。

Optionally, in the step S4, the first time is 1-3 h.

In this embodiment, for example, but not limiting of, the time period for collecting the gas is 2 hours.

Alternatively, in the step S3, the adsorbent is 4A molecular sieve or 5A molecular sieve; and/or the presence of a gas in the gas,

in the step S3, the adsorption temperature in the adsorption device is less than or equal to 40 ℃.

Optionally, the sulfur in step S1 is in powder form; and/or the presence of a gas in the gas,

the purity of the sulfur is greater than or equal to 95%.

In this embodiment, for example, but not limited to, the mesh number of the sulfur powder in the step S1 is 10 to 800 meshes. For example, but not limited to, the sulfur has a purity of 99.9%.

Optionally, in the step S5, the second temperature is-30 to-20 ℃; and/or the presence of a gas in the gas,

the second pressure is-0.05 to-0.08 MPa.

Optionally, in the step S6, the third temperature is-55 to-45 ℃; and/or the presence of a gas in the gas,

the third pressure is-0.05 to-0.06 MPa.

To better illustrate the technical effects of the process for preparing high-purity hydrogen sulfide provided by the present invention, the present invention provides the following data for illustration. It should be understood that the data set forth in the following examples are merely intended to better illustrate the technical effect of the continuous process for the production of high purity chlorine gas as set forth in the present invention and are not to be construed as being equivalent to all experimental data.