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Preparation process of high-purity hydrogen sulfide

A preparation process, hydrogen sulfide technology, applied in the direction of hydrogen sulfide, sulfur compounds, inorganic chemistry, etc., can solve the problems such as the inability to realize industrial production, and achieve the effect of stable product gas quality, high degree of self-control, and easy control and operation of the process

Active Publication Date: 2021-09-14
TAIHE GAS JINGZHOU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Aiming at the deficiencies in the prior art, the present invention provides a high-purity hydrogen sulfide preparation process to solve the technical problem in the related art that the traditional high-purity hydrogen sulfide preparation cannot realize industrial production

Method used

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Examples

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Effect test

preparation example Construction

[0030] The present invention provides a process for preparing high purity hydrogen sulfide, the preparation process comprises the step of:

[0031] Step S1, the sulfur sequentially, the organic solvent and 1,2-bis (diphenylphosphino) ethane added to the kettle, mixing stirring, heating to a first temperature to the sulfur melted into a liquid to obtain a liquid melt;

[0032] Step S2, in step S1 to the melt introduced into the hydrogen, the reaction gas is collected, crude hydrogen sulfide;

[0033] Step S3, the crude product prepared in step S2 through the hydrogen sulfide into the adsorption device, and dried to give a low moisture hydrogen sulfide;

[0034] Step S4, step S3 low moisture obtained crude hydrogen sulfide into the tank, collecting the first time, to obtain the collection of hydrogen sulfide;

[0035] Step S5, the step S4 of hydrogen sulfide was collected into a product tank, removal of heavies impurities at a second temperature and a second pressure, to obtain a hy...

Embodiment 1

[0063] 1, experimental operation: First, in the reaction kettle were added sulfur 50kg, 250kg m-xylene and 50g 1,2- bis (diphenylphosphino) ethane, 30 to 40 strokes / min with stirring, and the reactor evacuated to a pressure of -0.01 MPa or, stirring until homogeneous, to obtain kneaded product; then, controlling the reaction temperature of the autoclave was 50 ℃, the reaction pressure was 0.05MPa, for the mix was heated to obtain a liquid melt; secondly, to the liquid melt to 5m 3 / H of high purity hydrogen gas flow rate into the hydrogen cylinder outlet pressure 0.1MPa, to effect a reaction between hydrogen and sulfur, the reaction gas was collected to give the crude sulfide; again, the crude product obtained above was loaded into hydrogen sulfide 4A molecular sieves adsorbing means has in addition to water and dried, to obtain low water sulfide; again after the low moisture after adsorption of hydrogen sulfide into the tank and a crude product was collected 3h, too collect hy...

Embodiment 2

[0066] 1, experimental operation: First, in the reaction kettle were added sulfur 50kg, 400kg m-xylene and 50g 1,2- bis (diphenylphosphino) ethane, 30 to 40 strokes / min with stirring, and the reactor evacuated to a pressure of -0.01 MPa or, stirring until homogeneous, to obtain kneaded product; then, controlling the reaction temperature of the autoclave was 60 ℃, the reaction pressure was 0.05MPa, for the mix was heated to obtain a liquid melt; secondly, to the liquid melt to 7.5m 3 / H of high purity hydrogen gas flow rate into the hydrogen cylinder outlet pressure 0.1MPa, to effect a reaction between hydrogen and sulfur, the reaction gas was collected to give the crude sulfide; again, the crude product obtained above was loaded into hydrogen sulfide suction means has 5A molecular sieves, drying to remove water, hydrogen sulfide have low water; then, the low hydrogen sulfide after the water adsorbed into the tank and a crude product was collected 2h, collecting too sulfide, whe...

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Abstract

The invention provides a process for preparing high-purity hydrogen sulfide, comprising: step S1, sequentially adding sulfur, organic solvent and 1,2-bis(diphenylphosphine)ethane into the reaction kettle, stirring and mixing, and using the first Heating at a heating temperature until the sulfur is melted into a liquid state to obtain a liquid melt; step S2, passing hydrogen gas into the melt, reacting and collecting the gas, and obtaining crude hydrogen sulfide; step S3, passing the crude hydrogen sulfide into the adsorption device, dry to obtain low-moisture hydrogen sulfide; step S4, pass low-moisture hydrogen sulfide into the crude product tank, and collect hydrogen sulfide at the first time; step S5, pass the collected hydrogen sulfide into the first-level finished product tank, Remove the heavy component impurities at the second temperature and the second pressure to obtain primary hydrogen sulfide; step S6, pass the primary hydrogen sulfide into the secondary finished product tank, and remove light components at the third temperature and the third pressure Separation of impurities to obtain high-purity hydrogen sulfide. The technical problem that the traditional high-purity hydrogen sulfide preparation process cannot be industrialized is solved.

Description

Technical field [0001] The present invention relates to the preparation of high purity gas technologies, and in particular the process relates to the preparation of high purity hydrogen sulfide. Background technique [0002] Hydrogen sulfide is an important chemical raw materials, mainly for the synthesis of fine organic chemicals, and inorganic salts, such as pesticides, Manufacture of pharmaceuticals, and various industrial refining of metal reagents and the like. In the related art, a variety of hydrogen sulfide in the synthesis method: First, the solvent method, the liquid sulfur is dissolved in a solvent, to which was fed hydrogen to produce hydrogen sulfide gas, the pre-reaction method, although good, but as the reaction of for the solvent to produce coking phenomenon, so that the reaction efficiency is reduced, it is difficult to realize industrial production; second is the use of sulfur vapor and hydrogen sulfide gas direct synthesis, although the method is simple, but th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B17/16
CPCC01B17/162C01B17/168
Inventor 曾令军汪正宏阳辉曾令霞
Owner TAIHE GAS JINGZHOU
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