CN104071758A - Device and method for preparing sodium hydrosulfide - Google Patents
Device and method for preparing sodium hydrosulfide Download PDFInfo
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- CN104071758A CN104071758A CN201410333401.9A CN201410333401A CN104071758A CN 104071758 A CN104071758 A CN 104071758A CN 201410333401 A CN201410333401 A CN 201410333401A CN 104071758 A CN104071758 A CN 104071758A
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Abstract
The invention discloses a device and a method for preparing sodium hydrosulfide by using sodium hydroxide to absorb hydrogen sulfide. The device comprises a carbon removing device and a desulfuration device. The method using the device for preparing sodium hydrosulfide by using sodium hydroxide to absorb hydrogen sulfide comprises the following steps: firstly performing absorption and exclusion chromatography in carbon removing reactors; then absorbing CO2 circularly to complete a decarbonizing process; lastly completing a desulfuration process in desulfurization reactors. The device provided by the invention is low in investment, small in occupied area and high in absorption efficiency, and can remove more than 99.9% of hydrogen sulfide, so that the content of hydrogen sulfide in tail gas can be reduced below 1 mg/Nm<3>, and the emission standards can be completely met.
Description
Technical field
The present invention relates to a kind of device and method of preparing Sodium sulfhydrate, be specifically related to a kind of device and preparation method who utilizes sodium hydroxide absorbing hydrogen sulphide to prepare Sodium sulfhydrate, belong to the high density acid gas field that absorption cycle gas sweetening unit extracting tower resolution gas forms.
Background technology
High density acid gas refers to containing H
2s 50% ~ 90%, CO
2gas 10% ~ 50%.The formation of high density acid gas, generally by take weakly alkaline solution as lyosorption (alcamines, Benfield, sulfone amine etc.), the acid gas component or the reaction that absorb in gas form compound, when raising, absorb rich solution temperature or reduce while resolving pressure, sulfur removing pregnant solution discharges sour gas (is mainly H
2s and CO
2) and the high density H of formation
2the gas of S.
Generally adopt at present the high concentrated acid gas of acid-making process and Crouse sulphur art breading processed, these two kinds of Technology mature and reliable, at petrochemical enterprise, extensively adopt, but the shortcoming such as these two kinds of Technologies exist that investment is high, occupation area of equipment large, the domestic value of the product that cannot provide, produce secondary pollution source tail-gas, generation of the related accessory of equipment is low.A part of enterprise adopts the method for altitude combustion to process high density acid gas in addition, and this method is not only wasted resource, and has caused serious topsoil.Along with the attention of country to environmental issue, within nearly 2 years, by the form of legislation, improve the standard of discharge, so adopt the method relevant enterprise of altitude combustion all to face the problem of time limit rectification.
The traditional technology of producing Sodium Sulphide is the method that adopts coal reduction mirabilite method, this method is that coal dust and saltcake batch mixing are heated to 900 ℃ of left and right in high-temperature calcination stove, in process, can generate Sodium Sulphide solid, this method is applicable to producing a large amount of Sodium Sulphide products, but this technique can cause severe contamination to environment.
Producing sulphur hydride alkaline traditional technology is to utilize high-magnesium brine to react with Sodium Sulphide, generate hydrogen sulfide, use again certain density Sodium Sulphide absorbing hydrogen sulphide gas, generate liquid sulfur sodium hydride, through operations such as sedimentation, evaporation, film-makings, obtain finished product Sodium sulfhydrate again, this method is applicable to a large amount of sulphur hydride alkaline products of producing, but the bittern metal ion content of this technique use easily exceeds standard, and product select quality rate is low.
Summary of the invention
For the technical problem of above-mentioned existence, the invention provides a kind of device of preparing Sodium sulfhydrate, this plant investment is few, floor space is little, assimilated efficiency is high, product Sodium sulfhydrate concentration is adjustable, exhaust emissions is completely up to standard, three-waste free discharge, economic worth are high.
The technical solution used in the present invention is:
A kind of device of preparing Sodium sulfhydrate, comprise carbon removing device and desulfurizer, described carbon removing device comprises that one-level is removed carbon reactor, secondary removes carbon reactor, one-level de-carbon recycle pump, secondary de-carbon recycle pump, described desulfurizer comprises first grade desulfurizing reactor, two-grade desulfurizing reactor, three grades of desulphurization reactors, first grade desulfurizing recycle pump, two-grade desulfurizing recycle pump and three grades of desulfuration recycle pumps, and described one-level is except carbon reactor, secondary are except being communicated with successively between carbon reactor, first grade desulfurizing reactor, two-grade desulfurizing reactor and three grades of desulphurization reactors.
The present invention also provides a kind of method of preparing Sodium sulfhydrate, and the related principles of chemistry are as follows:
Absorption reaction: 2NaOH+H
2s → Na
2s+H
2o
Product formation reaction: Na
2s+H
2s → 2NaHS
Byproduct formation reaction: NaOH+CO
2→ NaHCO
3
Row analyses reaction: CO
2+ NaHS+ H
2o → NaHCO
3+ H
2s ↑
Preparation method comprises the following steps:
A, contain H
2s and CO
2the acid gas of gas removes carbon reactor top from one-level and enters reactor, to secondary, except in carbon reactor, add sodium hydroxide solution continuously simultaneously, alkali lye in sodium hydroxide solution and secondary carbon dioxide cleaner enters secondary and carries out absorption reaction except carbon reactor after secondary de-carbon recycle pump stirs, reaction times is 15-60min, reacted solution enters through liquid level adjusting the one-level that contains balanced solution and analyses reaction except arranging in carbon reactor, and the reaction times is 60-300min;
B, one-level absorb CO except the balanced solution forming in carbon reactor turns back to one-level after one-level de-carbon recycle pump except circulating in carbon reactor
2gas, the CO of absorption
2gas is usingd the form of sodium hydrogen carbonate solution and is existed and as byproduct solution, complete carbon rejection process;
C, remove portion CO
2the acid gas of gas enters first grade desulfurizing reactor successively, two-grade desulfurizing reactor, three grades of desulphurization reactors, while excessive sodium hydrate solution enters three grades of desulphurization reactors through three grades of desulfuration recycle pumps and carries out absorption reaction together with acid gas, reaction times is 15-60min, reacted solution enters two-grade desulfurizing reactor through liquid level adjusting and carries out the reaction of product generation cycle, reaction times is 15-60min, the rear solution of reaction enters first grade desulfurizing reactor through liquid level adjusting again and carries out product formation reaction, reaction times is 15-60min, after discharging by first grade desulfurizing recycle pump side line through the reacted solution of A reactor, carry out concentration, make sodium hydrosulfide or Sodium sulfhydrate solid, complete sweetening process,
Balanced solution in described steps A, B is the NaHCO by 40-85% by mass ratio
3, the NaHS of 5-30% is, the Na of 5-30%
2cO
3with mixing of the NaOH of 5-20%.
In described steps A, secondary is except sodium hydroxide solution in carbon reactor and H
2s gas generation absorption reaction generates Na
2s or NaHS.
In described steps A, one-level is except NaHS in carbon reactor and CO
2there is row and analyse reaction generation NaHCO in gas
3and H
2s gas.
Sodium hydroxide solution and H in three grades of desulphurization reactors in described step C
2s gas generation absorption reaction generates Na
2s or NaHS; Na in described two-grade desulfurizing reactor
2s and H
2the formation reaction of S gas generation product generates NaHS; Na in described first grade desulfurizing reactor
2s and H
2the formation reaction of S gas generation product generates NaHS.
The process that described secondary removes the process of carbon reactor, the process of the reverse inflow two-grade desulfurizing of the solution reactor in described three grades of desulphurization reactors and the reverse inflow first grade desulfurizing of the solution reactor in two-grade desulfurizing reactor except the reverse inflow one-level of solution in carbon reactor is all to control to realize by level chain.
Reaction is to absorb or swirling flow atomizing absorbs by injection in described five reactors.
The external heating mode of the interior type of heating of concentration employing chuck heating or single-action, multiple-effect evaporator in described step C.
The invention has the beneficial effects as follows:
(1) the present invention adopts the direct absorbing hydrogen sulphide of sodium hydroxide, and in conjunction with proprietary device, absorption process belongs to typical acid-base reaction, is irreversible reaction, reacts completely rapidly, without discharging of waste liquid;
(2) plant investment of the present invention is few, floor space is little, assimilated efficiency is high;
(3) main products of the present invention be 40% ~ 80% adjustable Sodium sulfhydrate aqueous solution of strength of solution or purity at more than 98% Sodium sulfhydrate solid phase prod, byproduct is solid sodium carbonate, product economy is worth high;
(4) the present invention can remove more than 99.9% hydrogen sulfide, and in tail gas, hydrogen sulfide content discharge value can be down to below 1mg/Nm3, completely qualified discharge.
Accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention;
In figure: 1 one-level is except carbon reactor, and 2 secondarys are except carbon reactor, 3 first grade desulfurizing reactors, 4 two-grade desulfurizing reactors, 5 three grades of desulphurization reactors, 6 one-level de-carbon recycle pumps, 7 secondary de-carbon recycle pumps, 8 first grade desulfurizing recycle pumps, 9 two-grade desulfurizing recycle pumps, 10 3 grades of desulfuration recycle pumps.
Embodiment
Below the present invention is described in further detail.
As shown in Figure 1, a kind of device of preparing Sodium sulfhydrate, comprise carbon removing device and desulfurizer, described carbon removing device comprises that one-level removes carbon reactor 1, secondary is except carbon reactor 2, one-level de-carbon recycle pump 6, secondary de-carbon recycle pump 7, described desulfurizer comprises first grade desulfurizing reactor 3, two-grade desulfurizing reactor 4, three grades of desulphurization reactors 5, first grade desulfurizing recycle pump 8, two-grade desulfurizing recycle pump 9 and three grades of desulfuration recycle pumps 10, described one-level is except carbon reactor 1, secondary is except carbon reactor 2, first grade desulfurizing reactor 3, between two-grade desulfurizing reactor 4 and three grades of desulphurization reactors 5, be communicated with successively.
embodiment 1
A method of preparing Sodium sulfhydrate, comprises the following steps:
A, contain H
2s and CO
2the acid gas of gas removes carbon reactor 1 top from one-level and enters reactor, to secondary, except in carbon reactor 2, add sodium hydroxide solution continuously, the alkali lye in sodium hydroxide solution and secondary carbon dioxide cleaner 2 enters secondary and generates Na except carbon reactor 2 carries out absorption reaction after secondary de-carbon recycle pump 7 stirs simultaneously
2s or NaHS, the reaction times is 15min, reacted solution enters through liquid level adjusting the one-level that contains balanced solution and analyses reaction generation NaHCO except arranging in carbon reactor 1
3and H
2s gas, the reaction times is 60min;
The balanced solution that B, one-level are removed carbon reactor 1 interior formation turns back to one-level except circulation absorption CO in carbon reactor 1 after one-level de-carbon recycle pump 6
2gas, the CO of absorption
2gas is usingd the form of sodium hydrogen carbonate solution and is existed and as byproduct solution, complete carbon rejection process;
C, remove portion CO
2the acid gas of gas enters first grade desulfurizing reactor 3, two-grade desulfurizing reactor 4, three grades of desulphurization reactors 5 successively, and excessive sodium hydrate solution enters three grades of desulphurization reactors 5 through three grades of desulfuration recycle pumps 10 and carries out absorption reaction and generate Na together with acid gas simultaneously
2s or NaHS, reaction times is 15min, reacted solution enters two-grade desulfurizing reactor 4 through liquid level adjusting and carries out product generation cycle reaction generation NaHS, reaction times is 15min, the rear solution of reaction enters first grade desulfurizing reactor 3 through liquid level adjusting again and carries out product formation reaction generation NaHS, reaction times is 15min, after discharging by first grade desulfurizing recycle pump 8 side lines through the reacted solution of A reactor, carry out concentration, make sodium hydrosulfide or Sodium sulfhydrate solid, complete sweetening process;
Balanced solution in described steps A, B is by 40% NaHCO by mass ratio
3, 20% NaHS, 15% Na
2cO
3with mixing of 25% NaOH.
The process that described secondary removes the process of carbon reactor 1, the process of the reverse inflow two-grade desulfurizing of the solution reactor 4 in described three grades of desulphurization reactors 5 and the reverse inflow first grade desulfurizing of the solution reactor 3 in two-grade desulfurizing reactor 4 except the reverse inflow one-level of solution in carbon reactor 2 is all to control to realize by level chain.Reaction is to absorb or swirling flow atomizing absorbs by injection in described five reactors.The external heating mode of the interior type of heating of concentration employing chuck heating or single-action, multiple-effect evaporator in described step C.
embodiment 2
A method of preparing Sodium sulfhydrate, comprises the following steps:
A, contain H
2s and CO
2the acid gas of gas removes carbon reactor 1 top from one-level and enters reactor, to secondary, except in carbon reactor 2, add sodium hydroxide solution continuously, the alkali lye in sodium hydroxide solution and secondary carbon dioxide cleaner 2 enters secondary and generates Na except carbon reactor 2 carries out absorption reaction after secondary de-carbon recycle pump 7 stirs simultaneously
2s or NaHS, the reaction times is 20min, reacted solution enters through liquid level adjusting the one-level that contains balanced solution and analyses reaction generation NaHCO except arranging in carbon reactor 1
3and H
2s gas, the reaction times is 180min;
The balanced solution that B, one-level are removed carbon reactor 1 interior formation turns back to one-level except circulation absorption CO in carbon reactor 1 after one-level de-carbon recycle pump 6
2gas, the CO of absorption
2gas is usingd the form of sodium hydrogen carbonate solution and is existed and as byproduct solution, complete carbon rejection process;
C, remove portion CO
2the acid gas of gas enters first grade desulfurizing reactor 3, two-grade desulfurizing reactor 4, three grades of desulphurization reactors 5 successively, and excessive sodium hydrate solution enters three grades of desulphurization reactors 5 through three grades of desulfuration recycle pumps 10 and carries out absorption reaction and generate Na together with acid gas simultaneously
2s or NaHS, reaction times is 25min, reacted solution enters two-grade desulfurizing reactor 4 through liquid level adjusting and carries out product generation cycle reaction generation NaHS, reaction times is 45min, the rear solution of reaction enters first grade desulfurizing reactor 3 through liquid level adjusting again and carries out product formation reaction generation NaHS, reaction times is 30min, after discharging by first grade desulfurizing recycle pump 8 side lines through the reacted solution of A reactor, carry out concentration, make sodium hydrosulfide or Sodium sulfhydrate solid, complete sweetening process;
Balanced solution in described steps A, B is by 50% NaHCO by mass ratio
3, 30% NaHS, 15% Na
2cO
3with mixing of 5% NaOH.
The process that described secondary removes the process of carbon reactor 1, the process of the reverse inflow two-grade desulfurizing of the solution reactor 4 in described three grades of desulphurization reactors 5 and the reverse inflow first grade desulfurizing of the solution reactor 3 in two-grade desulfurizing reactor 4 except the reverse inflow one-level of solution in carbon reactor 2 is all to control to realize by level chain.Reaction is to absorb or swirling flow atomizing absorbs by injection in described five reactors.The external heating mode of the interior type of heating of concentration employing chuck heating or single-action, multiple-effect evaporator in described step C.
embodiment 3
A method of preparing Sodium sulfhydrate, comprises the following steps:
A, contain H
2s and CO
2the acid gas of gas removes carbon reactor 1 top from one-level and enters reactor, to secondary, except in carbon reactor 2, add sodium hydroxide solution continuously, the alkali lye in sodium hydroxide solution and secondary carbon dioxide cleaner 2 enters secondary and generates Na except carbon reactor 2 carries out absorption reaction after secondary de-carbon recycle pump 7 stirs simultaneously
2s or NaHS, the reaction times is 45min, reacted solution enters through liquid level adjusting the one-level that contains balanced solution and analyses reaction generation NaHCO except arranging in carbon reactor 1
3and H
2s gas, the reaction times is 120min;
The balanced solution that B, one-level are removed carbon reactor 1 interior formation turns back to one-level except circulation absorption CO in carbon reactor 1 after one-level de-carbon recycle pump 6
2gas, the CO of absorption
2gas is usingd the form of sodium hydrogen carbonate solution and is existed and as byproduct solution, complete carbon rejection process;
C, remove portion CO
2the acid gas of gas enters first grade desulfurizing reactor 3, two-grade desulfurizing reactor 4, three grades of desulphurization reactors 5 successively, and excessive sodium hydrate solution enters three grades of desulphurization reactors 5 through three grades of desulfuration recycle pumps 10 and carries out absorption reaction and generate Na together with acid gas simultaneously
2s or NaHS, reaction times is 40min, reacted solution enters two-grade desulfurizing reactor 4 through liquid level adjusting and carries out product generation cycle reaction generation NaHS, reaction times is 30min, the rear solution of reaction enters first grade desulfurizing reactor 3 through liquid level adjusting again and carries out product formation reaction generation NaHS, reaction times is 50min, after discharging by first grade desulfurizing recycle pump 8 side lines through the reacted solution of A reactor, carry out concentration, make sodium hydrosulfide or Sodium sulfhydrate solid, complete sweetening process;
Balanced solution in described steps A, B is by 55% NaHCO by mass ratio
3, 10% NaHS, 25% Na
2cO
3with mixing of 10% NaOH.
The process that described secondary removes the process of carbon reactor 1, the process of the reverse inflow two-grade desulfurizing of the solution reactor 4 in described three grades of desulphurization reactors 5 and the reverse inflow first grade desulfurizing of the solution reactor 3 in two-grade desulfurizing reactor 4 except the reverse inflow one-level of solution in carbon reactor 2 is all to control to realize by level chain.Reaction is to absorb or swirling flow atomizing absorbs by injection in described five reactors.The external heating mode of the interior type of heating of concentration employing chuck heating or single-action, multiple-effect evaporator in described step C.
embodiment 4
A method of preparing Sodium sulfhydrate, comprises the following steps:
A, contain H
2s and CO
2the acid gas of gas removes carbon reactor 1 top from one-level and enters reactor, to secondary, except in carbon reactor 2, add sodium hydroxide solution continuously, the alkali lye in sodium hydroxide solution and secondary carbon dioxide cleaner 2 enters secondary and generates Na except carbon reactor 2 carries out absorption reaction after secondary de-carbon recycle pump 7 stirs simultaneously
2s or NaHS, the reaction times is 55min, reacted solution enters through liquid level adjusting the one-level that contains balanced solution and analyses reaction generation NaHCO except arranging in carbon reactor 1
3and H
2s gas, the reaction times is 240min;
The balanced solution that B, one-level are removed carbon reactor 1 interior formation turns back to one-level except circulation absorption CO in carbon reactor 1 after one-level de-carbon recycle pump 6
2gas, the CO of absorption
2gas is usingd the form of sodium hydrogen carbonate solution and is existed and as byproduct solution, complete carbon rejection process;
C, remove portion CO
2the acid gas of gas enters first grade desulfurizing reactor 3, two-grade desulfurizing reactor 4, three grades of desulphurization reactors 5 successively, and excessive sodium hydrate solution enters three grades of desulphurization reactors 5 through three grades of desulfuration recycle pumps 10 and carries out absorption reaction and generate Na together with acid gas simultaneously
2s or NaHS, reaction times is 35min, reacted solution enters two-grade desulfurizing reactor 4 through liquid level adjusting and carries out product generation cycle reaction generation NaHS, reaction times is 40min, the rear solution of reaction enters first grade desulfurizing reactor 3 through liquid level adjusting again and carries out product formation reaction generation NaHS, reaction times is 40min, after discharging by first grade desulfurizing recycle pump 8 side lines through the reacted solution of A reactor, carry out concentration, make sodium hydrosulfide or Sodium sulfhydrate solid, complete sweetening process;
Balanced solution in described steps A, B is by 60% NaHCO by mass ratio
3, 5% NaHS, 30% Na
2cO
3with mixing of 5% NaOH.
The process that described secondary removes the process of carbon reactor 1, the process of the reverse inflow two-grade desulfurizing of the solution reactor 4 in described three grades of desulphurization reactors 5 and the reverse inflow first grade desulfurizing of the solution reactor 3 in two-grade desulfurizing reactor 4 except the reverse inflow one-level of solution in carbon reactor 2 is all to control to realize by level chain.Reaction is to absorb or swirling flow atomizing absorbs by injection in described five reactors.The external heating mode of the interior type of heating of concentration employing chuck heating or single-action, multiple-effect evaporator in described step C.
embodiment 5
A method of preparing Sodium sulfhydrate, comprises the following steps:
A, contain H
2s and CO
2the acid gas of gas removes carbon reactor 1 top from one-level and enters reactor, to secondary, except in carbon reactor 2, add sodium hydroxide solution continuously, the alkali lye in sodium hydroxide solution and secondary carbon dioxide cleaner 2 enters secondary and generates Na except carbon reactor 2 carries out absorption reaction after secondary de-carbon recycle pump 7 stirs simultaneously
2s or NaHS, the reaction times is 40min, reacted solution enters through liquid level adjusting the one-level that contains balanced solution and analyses reaction generation NaHCO except arranging in carbon reactor 1
3and H
2s gas, the reaction times is 120min;
The balanced solution that B, one-level are removed carbon reactor 1 interior formation turns back to one-level except circulation absorption CO in carbon reactor 1 after one-level de-carbon recycle pump 6
2gas, the CO of absorption
2gas is usingd the form of sodium hydrogen carbonate solution and is existed and as byproduct solution, complete carbon rejection process;
C, remove portion CO
2the acid gas of gas enters first grade desulfurizing reactor 3, two-grade desulfurizing reactor 4, three grades of desulphurization reactors 5 successively, and excessive sodium hydrate solution enters three grades of desulphurization reactors 5 through three grades of desulfuration recycle pumps 10 and carries out absorption reaction and generate Na together with acid gas simultaneously
2s or NaHS, reaction times is 30min, reacted solution enters two-grade desulfurizing reactor 4 through liquid level adjusting and carries out product generation cycle reaction generation NaHS, reaction times is 20min, the rear solution of reaction enters first grade desulfurizing reactor 3 through liquid level adjusting again and carries out product formation reaction generation NaHS, reaction times is 35min, after discharging by first grade desulfurizing recycle pump 8 side lines through the reacted solution of A reactor, carry out concentration, make sodium hydrosulfide or Sodium sulfhydrate solid, complete sweetening process;
Balanced solution in described steps A, B is by 85% NaHCO by mass ratio
3, 10% NaHS, 10% Na
2cO
3with mixing of 15% NaOH.
The process that described secondary removes the process of carbon reactor 1, the process of the reverse inflow two-grade desulfurizing of the solution reactor 4 in described three grades of desulphurization reactors 5 and the reverse inflow first grade desulfurizing of the solution reactor 3 in two-grade desulfurizing reactor 4 except the reverse inflow one-level of solution in carbon reactor 2 is all to control to realize by level chain.Reaction is to absorb or swirling flow atomizing absorbs by injection in described five reactors.The external heating mode of the interior type of heating of concentration employing chuck heating or single-action, multiple-effect evaporator in described step C.
embodiment 6
A method of preparing Sodium sulfhydrate, comprises the following steps:
A, contain H
2s and CO
2the acid gas of gas removes carbon reactor 1 top from one-level and enters reactor, to secondary, except in carbon reactor 2, add sodium hydroxide solution continuously, the alkali lye in sodium hydroxide solution and secondary carbon dioxide cleaner 2 enters secondary and generates Na except carbon reactor 2 carries out absorption reaction after secondary de-carbon recycle pump 7 stirs simultaneously
2s or NaHS, the reaction times is 35min, reacted solution enters through liquid level adjusting the one-level that contains balanced solution and analyses reaction generation NaHCO except arranging in carbon reactor 1
3and H
2s gas, the reaction times is 180min;
The balanced solution that B, one-level are removed carbon reactor 1 interior formation turns back to one-level except circulation absorption CO in carbon reactor 1 after one-level de-carbon recycle pump 6
2gas, the CO of absorption
2gas is usingd the form of sodium hydrogen carbonate solution and is existed and as byproduct solution, complete carbon rejection process;
C, remove portion CO
2the acid gas of gas enters first grade desulfurizing reactor 3, two-grade desulfurizing reactor 4, three grades of desulphurization reactors 5 successively, and excessive sodium hydrate solution enters three grades of desulphurization reactors 5 through three grades of desulfuration recycle pumps 10 and carries out absorption reaction and generate Na together with acid gas simultaneously
2s or NaHS, reaction times is 20min, reacted solution enters two-grade desulfurizing reactor 4 through liquid level adjusting and carries out product generation cycle reaction generation NaHS, reaction times is 50min, the rear solution of reaction enters first grade desulfurizing reactor 3 through liquid level adjusting again and carries out product formation reaction generation NaHS, reaction times is 45min, after discharging by first grade desulfurizing recycle pump 8 side lines through the reacted solution of A reactor, carry out concentration, make sodium hydrosulfide or Sodium sulfhydrate solid, complete sweetening process;
Balanced solution in described steps A, B is by 70% NaHCO by mass ratio
3, 20% NaHS, 5% Na
2cO
3with mixing of 5% NaOH.
The process that described secondary removes the process of carbon reactor 1, the process of the reverse inflow two-grade desulfurizing of the solution reactor 4 in described three grades of desulphurization reactors 5 and the reverse inflow first grade desulfurizing of the solution reactor 3 in two-grade desulfurizing reactor 4 except the reverse inflow one-level of solution in carbon reactor 2 is all to control to realize by level chain.Reaction is to absorb or swirling flow atomizing absorbs by injection in described five reactors.The external heating mode of the interior type of heating of concentration employing chuck heating or single-action, multiple-effect evaporator in described step C.
embodiment 7
A method of preparing Sodium sulfhydrate, comprises the following steps:
A, contain H
2s and CO
2the acid gas of gas removes carbon reactor 1 top from one-level and enters reactor, to secondary, except in carbon reactor 2, add sodium hydroxide solution continuously, the alkali lye in sodium hydroxide solution and secondary carbon dioxide cleaner 2 enters secondary and generates Na except carbon reactor 2 carries out absorption reaction after secondary de-carbon recycle pump 7 stirs simultaneously
2s or NaHS, the reaction times is 60min, reacted solution enters through liquid level adjusting the one-level that contains balanced solution and analyses reaction generation NaHCO except arranging in carbon reactor 1
3and H
2s gas, the reaction times is 300min;
The balanced solution that B, one-level are removed carbon reactor 1 interior formation turns back to one-level except circulation absorption CO in carbon reactor 1 after one-level de-carbon recycle pump 6
2gas, the CO of absorption
2gas is usingd the form of sodium hydrogen carbonate solution and is existed and as byproduct solution, complete carbon rejection process;
C, remove portion CO
2the acid gas of gas enters first grade desulfurizing reactor 3, two-grade desulfurizing reactor 4, three grades of desulphurization reactors 5 successively, and excessive sodium hydrate solution enters three grades of desulphurization reactors 5 through three grades of desulfuration recycle pumps 10 and carries out absorption reaction and generate Na together with acid gas simultaneously
2s or NaHS, reaction times is 60min, reacted solution enters two-grade desulfurizing reactor 4 through liquid level adjusting and carries out product generation cycle reaction generation NaHS, reaction times is 60min, the rear solution of reaction enters first grade desulfurizing reactor 3 through liquid level adjusting again and carries out product formation reaction generation NaHS, reaction times is 60min, after discharging by first grade desulfurizing recycle pump 8 side lines through the reacted solution of A reactor, carry out concentration, make sodium hydrosulfide or Sodium sulfhydrate solid, complete sweetening process;
Balanced solution in described steps A, B is by 80% NaHCO by mass ratio
3, 5% NaHS, 5% Na
2cO
3with mixing of 10% NaOH.
The process that described secondary removes the process of carbon reactor 1, the process of the reverse inflow two-grade desulfurizing of the solution reactor 4 in described three grades of desulphurization reactors 5 and the reverse inflow first grade desulfurizing of the solution reactor 3 in two-grade desulfurizing reactor 4 except the reverse inflow one-level of solution in carbon reactor 2 is all to control to realize by level chain.Reaction is to absorb or swirling flow atomizing absorbs by injection in described five reactors.The external heating mode of the interior type of heating of concentration employing chuck heating or single-action, multiple-effect evaporator in described step C.
Claims (8)
1. a device of preparing Sodium sulfhydrate, it is characterized in that, described device comprises carbon removing device and desulfurizer, described carbon removing device comprises that one-level removes carbon reactor (1), secondary is except carbon reactor (2), one-level de-carbon recycle pump (6), secondary de-carbon recycle pump (7), described desulfurizer comprises first grade desulfurizing reactor (3), two-grade desulfurizing reactor (4), three grades of desulphurization reactors (5), first grade desulfurizing recycle pump (8), two-grade desulfurizing recycle pump (9) and three grades of desulfuration recycle pumps (10), described one-level is except carbon reactor (1), secondary is except carbon reactor (2), first grade desulfurizing reactor (3), between two-grade desulfurizing reactor (4) and three grades of desulphurization reactors (5), be communicated with successively.
2. right to use requires device described in 1 to prepare a method for Sodium sulfhydrate, it is characterized in that, comprises the following steps:
A, contain H
2s and CO
2the acid gas of gas removes carbon reactor (1) top from one-level and enters reactor, to secondary, except in carbon reactor (2), add sodium hydroxide solution continuously simultaneously, alkali lye in sodium hydroxide solution and secondary carbon dioxide cleaner (2) enters secondary and carries out absorption reaction except carbon reactor (2) after secondary de-carbon recycle pump (7) stirs, reaction times is 15-60min, reacted solution enters through liquid level adjusting the one-level that contains balanced solution and analyses reaction except arranging in carbon reactor (1), and the reaction times is 60-300min;
B, one-level are removed circulation absorption CO in carbon reactor (1) except the interior balanced solution forming of carbon reactor (1) turns back to one-level after one-level de-carbon recycle pump (6)
2gas, the CO of absorption
2gas is usingd the form of sodium hydrogen carbonate solution and is existed and as byproduct solution, complete carbon rejection process;
C, remove portion CO
2the acid gas of gas enters first grade desulfurizing reactor (3) successively, two-grade desulfurizing reactor (4), three grades of desulphurization reactors (5), simultaneously excessive sodium hydrate solution enters together three grades of desulphurization reactors (5) through three grades of desulfuration recycle pumps (10) and acid gas and carries out absorption reaction, reaction times is 15-60min, reacted solution enters two-grade desulfurizing reactor (4) through liquid level adjusting and carries out the reaction of product generation cycle, reaction times is 15-60min, the rear solution of reaction enters first grade desulfurizing reactor (3) through liquid level adjusting again and carries out product formation reaction, reaction times is 15-60min, after discharging by first grade desulfurizing recycle pump (8) side line through the reacted solution of A reactor, carry out concentration, make sodium hydrosulfide or Sodium sulfhydrate solid, complete sweetening process,
Balanced solution in described steps A, B is the NaHCO by 40-85% by mass ratio
3, the NaHS of 5-30% is, the Na of 5-30%
2cO
3with mixing of the NaOH of 5-20%.
3. the method for preparing Sodium sulfhydrate according to claim 2, is characterized in that, in described steps A, secondary is except the interior sodium hydroxide solution of carbon reactor (2) and H
2s gas generation absorption reaction generates Na
2s or NaHS.
4. the method for preparing Sodium sulfhydrate according to claim 2, is characterized in that, in described steps A, one-level is except the interior NaHS of carbon reactor (1) and CO
2there is row and analyse reaction generation NaHCO in gas
3and H
2s gas.
5. the method for preparing Sodium sulfhydrate according to claim 2, is characterized in that, the interior sodium hydroxide solution of three grades of desulphurization reactors (5) and H in described step C
2s gas generation absorption reaction generates Na
2s or NaHS; The interior Na of described two-grade desulfurizing reactor (4)
2s and H
2the formation reaction of S gas generation product generates NaHS; The interior Na of described first grade desulfurizing reactor (3)
2s and H
2the formation reaction of S gas generation product generates NaHS.
6. the method for preparing Sodium sulfhydrate according to claim 2, it is characterized in that, the interior process of the reverse inflow two-grade desulfurizing of solution reactor (4) and the process of the reverse inflow first grade desulfurizing of the solution reactor (3) in two-grade desulfurizing reactor (4) of process, described three grades of desulphurization reactors (5) that described secondary removes carbon reactor (1) except the reverse inflow one-level of solution in carbon reactor (2) is all to control to realize by level chain.
7. the method for preparing Sodium sulfhydrate according to claim 2, is characterized in that, reaction is to absorb or swirling flow atomizing absorbs by injection in described five reactors.
8. the method for preparing Sodium sulfhydrate according to claim 2, is characterized in that, the external heating mode of the interior type of heating of concentration employing chuck heating or single-action, multiple-effect evaporator in described step C.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3839548A (en) * | 1972-10-13 | 1974-10-01 | Lion Oil Co | Process for producing sodium hydrosulfide solutions |
| CN102059038A (en) * | 2010-12-20 | 2011-05-18 | 聊城市鲁西化工工程设计有限责任公司 | Treatment process and device of waste gas containing hydrogen sulfide and carbon dioxide |
| CN103551018A (en) * | 2013-11-07 | 2014-02-05 | 中天环保产业(集团)有限公司 | Sulfur-containing tail gas purifying and recycling method |
| CN103693626A (en) * | 2013-12-18 | 2014-04-02 | 安徽工业大学 | Method for preparing sodium hydrosulfide from hydrogen sulfide acid gas containing carbon dioxide |
| CN203998955U (en) * | 2014-07-15 | 2014-12-10 | 袁磊 | A kind of device of preparing Sodium sulfhydrate |
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2014
- 2014-07-15 CN CN201410333401.9A patent/CN104071758A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3839548A (en) * | 1972-10-13 | 1974-10-01 | Lion Oil Co | Process for producing sodium hydrosulfide solutions |
| CN102059038A (en) * | 2010-12-20 | 2011-05-18 | 聊城市鲁西化工工程设计有限责任公司 | Treatment process and device of waste gas containing hydrogen sulfide and carbon dioxide |
| CN103551018A (en) * | 2013-11-07 | 2014-02-05 | 中天环保产业(集团)有限公司 | Sulfur-containing tail gas purifying and recycling method |
| CN103693626A (en) * | 2013-12-18 | 2014-04-02 | 安徽工业大学 | Method for preparing sodium hydrosulfide from hydrogen sulfide acid gas containing carbon dioxide |
| CN203998955U (en) * | 2014-07-15 | 2014-12-10 | 袁磊 | A kind of device of preparing Sodium sulfhydrate |
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