CN102765700A - Technique method for producing sodium bisulfide - Google Patents
Technique method for producing sodium bisulfide Download PDFInfo
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- CN102765700A CN102765700A CN201210286978XA CN201210286978A CN102765700A CN 102765700 A CN102765700 A CN 102765700A CN 201210286978X A CN201210286978X A CN 201210286978XA CN 201210286978 A CN201210286978 A CN 201210286978A CN 102765700 A CN102765700 A CN 102765700A
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Abstract
The invention discloses a technique method for producing sodium bisulfide and belongs to the technical field of the chemical engineering production technology. The technique method for producing sodium bisulfide is low in production cost and can control product quality easily during production. The technique method includes: feeding buffered hydrogen sulfide and process absorption liquid with sodium sulphide as the main ingredient into an absorption tower respectively from the lower portion and the upper portion of the absorption tower, absorbing the hydrogen sulfide and the process absorption liquid on the surface of packing in the absorption tower to generate solution with the sodium bisulfide as the main ingredient, enabling the solution to flow to the bottom of the absorption tower, and discharging the unabsorbed hydrogen sulfide tail gas from the top of the absorption tower; pumping the solution at the bottom of the absorption tower out, returning most of the solution back to the absorption tower for recycling, feeding the small amount of solution to a sodium bisulfide production solution storing tank, and simultaneously adding the process absorption liquid in the absorption tower from the upper portion of the absorption tower during the absorption circulating process; and finally performing evaporation, concentration and dehydration on the solution, cooling the solution for molding, packaging and finishing the production of the sodium bisulfide.
Description
Technical field
The present invention relates to a kind of process method of producing Sodium sulfhydrate, belong to Chemical Manufacture Technology field.
Background technology
Traditional Sodium sulfhydrate production technique is an interrupter method, and the production equipment of said interrupter method production technique is made up of equipment such as two or more absorption reactor thermallies, vacuum pump, alkali lye charge pump, sodium hydrosulfide extractor pumps, and absorption liquid is a sodium hydroxide solution.When concrete production, its production process is following, at first gives the sodium hydroxide solution that adds set amount in certain absorption reactor thermally, closes related valve, starts whisking appliance and stirs, and starts vacuum pump and vacuumizes; , vacuum tightness feeds hydrogen sulfide when reaching set(ting)value, under agitation reaction to reactor drum; When reaction arrives latter stage, in order to guarantee in the reaction product not Containing Sulfur sodium, need to continue logical hydrogen sulfide, this moment, a large amount of hydrogen sulfide were extracted out by vacuum pump, sent into other reactor drum; Close the hydrogen sulfide intake valve when reaction finishes, under agitation continue to vacuumize, the hydrogen sulfide in the reactor drum dead space is all extracted out, turn off stirring, vacuum pump again; Open bleeder valve, start the Sodium sulfhydrate extractor pump, sodium hydrosulfide is extracted out.The operating process and the said process of other absorption reactor thermally are identical, and several absorption reactor thermallies hocket.
There is following shortcoming and defect in said traditional Sodium sulfhydrate interrupter method production technique:
1, power consumption is than higher, and major cause one is in order to guarantee hydrogen sulfide and the even absorption reaction of sodium hydroxide in the reactor drum, and whole absorption process stirs absorption liquid; The 2nd, hydrogen sulfide is hypertoxic gas, in case reveal, can cause a serious accident, and causes that personnel are poisoned to death, and therefore need under the condition that vacuumizes, carry out.The use of stirring and vacuum pump causes the power consumption of product bigger, and cost is high.
2, the bad control of quality product, owing to receive multiple factor affecting such as hydrogen sulfide fluctuations in discharge, envrionment temperature, stirring velocity, vacuum pump, the bad control of reaction end, reaction product sodium sulfide content often occurs and exceeds standard, and needs to replenish situation about absorbing.
3, be difficult to realize automated operation that operator's quantity is many, labor waste is serious.Because operation steps is many, the equipment start-stop is frequent, the reference mark is many etc., is difficult to the realization sequencing operate automatically, each step all needs personnel operation basically.
4, valve, stirring, pump are all operated frequently, cause equipment failure rate high, and the maintenance maintenance task is heavy.
5, environment stench, no matter be that reactor drum adopts separate unit or many tandems to absorb, hydrogen sulfide all can not be by thorough absorption, the hydrogen sulfide content in the absorption tail gas causes the Working environment stench than higher.
Summary of the invention
Technical problem to be solved by this invention is: provide a kind of production cost low, in the production process, quality product is the process method of the production Sodium sulfhydrate of control easily.
The technical scheme that adopts for solving the problems of the technologies described above is: a kind of process method of producing Sodium sulfhydrate, may further comprise the steps,
At first, the hydrogen sulfide virgin gas is sent into hydrogen sulfide surge tank buffering, and the preparation staple is the process absorption liquid of sodium sulphite;
Then; With hydrogen sulfide and the process absorption liquid after the buffering; Send into the absorption tower from the bottom and the top on absorption tower respectively, the filling surface of the hydrogen sulfide of rising in the absorption tower by spray and under the process absorption liquid absorb, generate sodium hydrosulfide; And flow at the bottom of the absorption Tata, unabsorbed hydrogen sulfide tail gas is discharged from the top, absorption tower;
Then, the sodium hydrosulfide at the bottom of the tower is extracted out, big portion returns the absorption tower from top, absorption tower again and recycles; And after the content of control sodium sulphite does not exceed standard; Wherein sub-fraction solution is sent into Sodium sulfhydrate product solution storage tank, mends to the circulation absorption process from top, absorption tower simultaneously and goes into corresponding process absorption liquid, so repeatedly circulation; Just successive has generated the sodium hydrosulfide that sodium sulfide content does not exceed standard, and is stored in Sodium sulfhydrate product solution storage tank;
At last, send down road evaporation concentration dehydration, cooling forming, packaging process, accomplish the production process of Sodium sulfhydrate the solution in the Sodium sulfhydrate product solution storage tank.
Further be, when the preparation staple is the process absorption liquid of sodium sulphite, undertaken by following step,
At first; Send into the reabsorber from the bottom and the top of reabsorber respectively with hydrogen sulfide tail gas with by the formulated raw material absorption liquid of sodium hydroxide; The filling surface of hydrogen sulfide in reabsorber in the hydrogen sulfide tail gas that rises is by spray and the absorption of raw material absorption liquid down; Generating staple is the aqueous solution of sodium sulphite and sodium hydroxide, and flows at the bottom of the reabsorber tower, and the unabsorbed tail gas that absorbs is again discharged from the reabsorber cat head;
Then, be that the aqueous solution of sodium sulphite and sodium hydroxide is extracted out at the bottom of tower with staple, major part is again as absorbent solution again; Send into the reabsorber from reabsorber top and to recycle, few part is mended the circulation absorption process on absorption tower from top, absorption tower as the process absorption liquid; Simultaneously; Mend to the recycling absorption process from reabsorber top and to go into the raw material absorption liquid, the preparation of process absorption liquid has just been accomplished in circulation according to this.
Further be; The tail gas of absorption again of discharging from the reabsorber top; Row absorbs to handle and just can be discharged in the atmosphere when needing further to hydrogen sulfide; The said absorption that absorbs tail gas is again handled and is undertaken by following step, earlier the said tail gas that absorbs is again sent in the alkali lye protective pot that initial absorption liquid is housed, and a small amount of hydrogen sulfide that absorbs again in the tail gas is further absorbed by initial absorption liquid; The unabsorbed tail gas that absorbs is again sent in the purification deodorizer that sorbent material is housed again, and sorbent material will absorb the thorough adsorption cleaning of the micro-hydrogen sulfide gas that contains in the tail gas again.
Further be that the initial absorption liquid that uses in the alkali lye protective pot is by the formulated in proportion aqueous sodium hydroxide solution of sodium hydroxide.
Further being, is used initial absorption liquid when absorption absorbs tail gas again in the alkali lye protective pot to absorbing the raw material absorption liquid that benefit is gone in the working cycle again, perhaps is by the formulated in proportion aqueous sodium hydroxide solution of sodium hydroxide.
Further be; The process absorption liquid of in absorbing working cycle, importing; Except the process absorption liquid that uses first for utilize by absorption tower self initial absorption liquid through absorb the working cycle preparation, mending the process absorption liquid of going into later on, to be the staple that absorbs the working cycle preparation again be the aqueous solution of sodium sulphite.
The invention has the beneficial effects as follows: through being the process absorption liquid of sodium sulphite, send in the absorption tower from the bottom and the top on absorption tower respectively hydrogen sulfide and staple, make upwards mobile hydrogen sulfide and spray and under the process absorption liquid; Contact on the filling surface in the absorption tower, and absorbed by the process absorption liquid, generating major ingredient is the solution of Sodium sulfhydrate; Flow to the bottom on absorption tower, then, again solution is extracted out at the bottom of tower; Major part is sent into the absorption tower from top, absorption tower again, continues and the stink damp precursor reactant, and after the content of sodium sulphite does not exceed standard in control solution; A spot of solution is sent into Sodium sulfhydrate product solution storage tank, get into road evaporation concentration dehydration down, cooling forming, packaging process, so repeatedly circulation; Constantly extract qualified Sodium sulfhydrate product solution out; Simultaneously, constantly mend new process absorption liquid, just accomplish the production process of Sodium sulfhydrate.Like this, in the whole process of production of Sodium sulfhydrate, no longer as prior art; Need big power consumption equipment such as whisking appliance, vacuum pump, only need to absorb column bottoms pump formation production cycle and get final product, thereby effectively reduced power consumption; The production cost of being born, and, in the production process; Can accomplish to check at any time the content of the sodium sulphite in the mixing solutions in the production process, when its content overproof, can make mixing solutions continue circulation; With absorbing hydrogen sulphide gas, sodium sulphite is further changed into Sodium sulfhydrate, and then better guarantee the quality of product.
Description of drawings
Fig. 1 is a kind of production technique principle flow chart of producing the process method of Sodium sulfhydrate of the present invention.
Be labeled as among the figure: absorption tower 1, Sodium sulfhydrate product solution storage tank 2, reabsorber 3, alkali lye protective pot 4, purification deodorizer 5.
Embodiment
As shown in Figure 1 is that a kind of production cost provided by the invention is low, and in the production process, quality product is the process method of the production Sodium sulfhydrate of control easily.Said process method may further comprise the steps,
At first, the hydrogen sulfide virgin gas is sent into hydrogen sulfide surge tank buffering, and the preparation staple is the process absorption liquid of sodium sulphite;
Then; With hydrogen sulfide and the process absorption liquid after the buffering; Send into the absorption tower 1 from the bottom and the top on absorption tower 1 respectively, the filling surface of the hydrogen sulfide of rising in the absorption tower by spray and under the process absorption liquid absorb, generate sodium hydrosulfide; And flow at the bottom of 1 tower of absorption tower, unabsorbed hydrogen sulfide tail gas is discharged from the top, absorption tower;
Then, the sodium hydrosulfide at the bottom of the tower is extracted out, big portion returns the absorption tower 1 from 1 top, absorption tower again and recycles; And after the content of control sodium sulphite does not exceed standard; Wherein sub-fraction solution is sent into Sodium sulfhydrate product solution storage tank 2, mends to the circulation absorption process from 1 top, absorption tower simultaneously and goes into corresponding process absorption liquid, so repeatedly circulation; Just successive has generated the sodium hydrosulfide that sodium sulfide content does not exceed standard, and is stored in Sodium sulfhydrate product solution storage tank 2;
At last, send down road evaporation concentration dehydration, cooling forming, packaging process, accomplish the production process of Sodium sulfhydrate the solution in the Sodium sulfhydrate product solution storage tank 2.
Above-mentionedly send in the absorption tower 1 from the bottom and the top on absorption tower 1 respectively through being the process absorption liquid of sodium sulphite with hydrogen sulfide and staple, make upwards mobile hydrogen sulfide and spray and under the process absorption liquid; Contact on the filling surface in absorption tower 1, and absorbed by the process absorption liquid, generating major ingredient is the mixing solutions of Sodium sulfhydrate; Flow to the bottom on absorption tower 1, then, again mixing solutions is extracted out at the bottom of tower; Major part is sent into the absorption tower 1 from 1 top, absorption tower again, continues and the stink damp precursor reactant, and behind the content of the sodium sulphite in the control mixing solutions; A spot of mixing solutions is sent into Sodium sulfhydrate product solution storage tank, get into road evaporation concentration dehydration down, cooling forming, packaging process, so repeatedly circulation; Constantly extract sodium sulfide content out and reach the Sodium sulfhydrate product solution that control requires; Simultaneously, constantly mend new process absorption liquid, just accomplish the production process of Sodium sulfhydrate.Like this, owing in the whole process of production of Sodium sulfhydrate,, need big power consumption equipment such as whisking appliance, vacuum pump, thereby effectively reduced power consumption, the production cost of being born no longer as prior art; Simultaneously, most importantly, in process of production; Can accomplish to check at any time the content of the sodium sulphite in the solution, when its content overproof, can make solution continue circulation; With absorbing hydrogen sulphide gas, sodium sulphite is further changed into Sodium sulfhydrate, and then better guarantee the quality of product.
In the above-mentioned embodiment, when the preparation staple is the process absorption liquid of sodium sulphite,, still can improve current consumption, increase production cost if adopt existing interrupter method to prepare.In order to reduce current consumption to greatest extent, reduce production costs, simultaneously, improve the quality product of the Sodium sulfhydrate in the Sodium sulfhydrate production cycle process in the absorption tower, when the preparation staple is the process absorption liquid of sodium sulphite, undertaken by following step,
At first; Send into the reabsorber 3 from the bottom and the top of reabsorber 3 respectively with hydrogen sulfide tail gas with by the formulated raw material absorption liquid of sodium hydroxide; The filling surface of hydrogen sulfide in reabsorber in the hydrogen sulfide tail gas that rises is by spray and the absorption of raw material absorption liquid down; Generating staple is the aqueous solution of sodium sulphite and sodium hydroxide, and flows at the bottom of reabsorber 3 towers, and the unabsorbed tail gas that absorbs is again discharged from reabsorber 3 cats head;
Then, be that the aqueous solution of sodium sulphite and sodium hydroxide is extracted out at the bottom of tower with staple, major part is again as absorbent solution again; Send into the reabsorber 3 from reabsorber 3 tops and to recycle, few part is mended the circulation absorption process on absorption tower 1 from 1 top, absorption tower as the process absorption liquid; Simultaneously; Mend to the recycling absorption process from reabsorber 3 tops and to go into the raw material absorption liquid, the preparation of process absorption liquid has just been accomplished in circulation according to this.
Adopt above-mentioned process step to prepare the process absorption liquid, also do not need big power consumption equipment such as whisking appliance, vacuum pump, thereby reach the purpose of effective reduction operation energy consumption.Simultaneously; After hydrogen sulfide tail gas absorbed through reabsorber 3, wherein most hydrogen sulfide were absorbed, and unabsorbed tail gas is as absorbing the discharge of tail gas from reabsorber 3 tops again; Also be postorder to purification, the deodorizing of sulfuration tail gas, and thoroughly be discharged in the ambient air and provide convenience.
In the above-mentioned enforcement side; For the tail gas of absorption again that reabsorber 3 is discharged; In the environment around the discharge of ability safety, environmental protection; The tail gas of absorption again of discharging from reabsorber 3 tops, row absorbs to handle and just can be discharged in the atmosphere when needing further to hydrogen sulfide, and the said absorption that absorbs tail gas is again handled and is undertaken by following step; Earlier the said tail gas that absorbs is again sent in the alkali lye protective pot 4 that initial absorption liquid is housed; The a small amount of hydrogen sulfide that absorbs again in the tail gas is further absorbed by initial absorption liquid, and the unabsorbed tail gas that absorbs is again sent in the purification deodorizer 5 that sorbent material is housed again, and sorbent material will absorb the thorough adsorption cleaning of the micro-hydrogen sulfide gas that contains in the tail gas again; Last just with exhaust emissions to around environment in.
In embodiment; In order to reduce production costs, still can utilize again through the hydrogen sulfide composition that absorbs the circulation recovery again, simultaneously; In absorbing working cycle, replenish new process absorption liquid again for ease, also mend the raw material absorption liquid in the working cycle to absorbing again for ease.The initial absorption liquid that uses in the said alkali lye protective pot 4 is by the formulated in proportion aqueous sodium hydroxide solution of sodium hydroxide; Mend the raw material absorption liquid of going in the working cycle to absorbing, used initial absorption liquid when absorbing tail gas again for the 4 interior absorptions of alkali lye protective pot perhaps is by the formulated in proportion aqueous sodium hydroxide solution of sodium hydroxide again; The process absorption liquid of in absorbing working cycle, importing; Except the process absorption liquid that uses first for self utilize by absorption tower 1 initial absorption liquid through absorb the working cycle preparation, mending the process absorption liquid of going into later on, to be the staple that absorbs the working cycle preparation again be the aqueous solution of sodium sulphite.Like this; Both the hydrogen sulfide composition that reclaims had been carried out utilizing again; Limit production cost low; Guaranteed safety, the operation that can make the Sodium sulfhydrate cyclic production process, sodium sulphite cyclic production process of the inventive method again and in each working cycle, mend respective liquid realizes robotization completely, guarantee production process continuously, stable and safety.
In sum, adopt process method of the present invention to produce Sodium sulfhydrate, the absorption of hydrogen sulfide continuously, stable, the Sodium sulfhydrate product can be continuously, stablize discharging.And quality product can obtain stable control.The whole process of production operating safety, reliable, Working environment is friendly.Running cost is low, and product is competitive.
Claims (6)
1. process method of producing Sodium sulfhydrate is characterized in that: may further comprise the steps,
At first, the hydrogen sulfide virgin gas is sent into hydrogen sulfide surge tank buffering, and the preparation staple is the process absorption liquid of sodium sulphite;
Then; With hydrogen sulfide and the process absorption liquid after the buffering; Send into the absorption tower (1) from the bottom and the top of absorption tower (1) respectively, the filling surface of the hydrogen sulfide of rising in the absorption tower by spray and under the process absorption liquid absorb, generate sodium hydrosulfide; And flow at the bottom of the tower of absorption tower (1), unabsorbed hydrogen sulfide tail gas is discharged from the top, absorption tower;
Then; Sodium hydrosulfide at the bottom of the tower is extracted out; Big portion returns the absorption tower (1) from top, absorption tower (1) again and recycles, and after the content of control sodium sulphite did not exceed standard, wherein sub-fraction solution was sent into Sodium sulfhydrate product solution storage tank (2); Mend to the circulation absorption process from top, absorption tower (1) simultaneously and go into corresponding process absorption liquid; Circulation so repeatedly, just successive has generated the sodium hydrosulfide that sodium sulfide content does not exceed standard, and is stored in Sodium sulfhydrate product solution storage tank (2);
At last, send down road evaporation concentration dehydration, cooling forming, packaging process, accomplish the production process of Sodium sulfhydrate the solution in the Sodium sulfhydrate product solution storage tank (2).
2. a kind of process method of producing Sodium sulfhydrate according to claim 1 is characterized in that: when the preparation staple is the process absorption liquid of sodium sulphite, undertaken by following step,
At first; Send into the reabsorber (3) from the bottom and the top of reabsorber (3) respectively with hydrogen sulfide tail gas with by the formulated raw material absorption liquid of sodium hydroxide; The filling surface of hydrogen sulfide in reabsorber in the hydrogen sulfide tail gas that rises is by spray and the absorption of raw material absorption liquid down; Generating staple is the aqueous solution of sodium sulphite and sodium hydroxide, and flows at the bottom of reabsorber (3) tower, and the unabsorbed tail gas that absorbs is again discharged from reabsorber (3) cat head;
Then, be that the aqueous solution of sodium sulphite and sodium hydroxide is extracted out at the bottom of tower with staple, major part is again as absorbent solution again; Send into the reabsorber (3) from reabsorber (3) top and to recycle, few part is mended the circulation absorption process on absorption tower (1) from top, absorption tower (1) as the process absorption liquid; Simultaneously; Mend to the recycling absorption process from reabsorber (3) top and to go into the raw material absorption liquid, the preparation of process absorption liquid has just been accomplished in circulation according to this.
3. a kind of process method of producing Sodium sulfhydrate according to claim 2; It is characterized in that: the tail gas of absorption again of discharging from reabsorber (3) top; Row absorbs to handle and just can be discharged in the atmosphere when needing further to hydrogen sulfide; The said absorption that absorbs tail gas is again handled and is undertaken by following step; Earlier the said tail gas that absorbs is again sent in the alkali lye protective pot (4) that initial absorption liquid is housed; The a small amount of hydrogen sulfide that absorbs again in the tail gas is further absorbed by initial absorption liquid, and the unabsorbed tail gas that absorbs is again sent in the purification deodorizer (5) that sorbent material is housed again, and sorbent material will absorb the thorough adsorption cleaning of the micro-hydrogen sulfide gas that contains in the tail gas again.
4. a kind of process method of producing Sodium sulfhydrate according to claim 3 is characterized in that: the initial absorption liquid that uses in the alkali lye protective pot (4) is by the formulated in proportion aqueous sodium hydroxide solution of sodium hydroxide.
5. according to claim 3 or 4 described a kind of process methodes of producing Sodium sulfhydrate; It is characterized in that: mend the raw material absorption liquid of going in the working cycle to absorbing again; Used initial absorption liquid when absorbing tail gas again for the interior absorption of alkali lye protective pot (4) perhaps is by the formulated in proportion aqueous sodium hydroxide solution of sodium hydroxide.
6. a kind of process method of producing Sodium sulfhydrate according to claim 5; It is characterized in that: the process absorption liquid of in absorbing working cycle, importing; Except the process absorption liquid that uses first for self utilize by absorption tower (1) initial absorption liquid through absorb the working cycle preparation, mending the process absorption liquid of going into later on, to be the staple that absorbs the working cycle preparation again be the aqueous solution of sodium sulphite.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103058227A (en) * | 2012-12-03 | 2013-04-24 | 北京化工大学 | Process and device for recovering sodium sulphide wastewater in barium sulphate production |
| 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 |
| CN104370783A (en) * | 2014-10-30 | 2015-02-25 | 天津河清化学工业有限公司 | Hydrogen sulfide recycling method and hydrogen sulfide recycling system for continuously producing mercaptoacetic acid by adopting sodium hydrosulfide method |
| CN104971597A (en) * | 2014-04-10 | 2015-10-14 | 中国石油化工股份有限公司 | Technical method and device of producing sodium hydrosulfide from acid gas |
| CN106744710A (en) * | 2017-01-20 | 2017-05-31 | 山东金典化工有限公司 | The method that continuity method produces NaHS |
| CN115212706A (en) * | 2022-07-11 | 2022-10-21 | 江苏楷鼎环保装备有限公司 | Tail gas treatment method for sulfur black dye production system |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103058227A (en) * | 2012-12-03 | 2013-04-24 | 北京化工大学 | Process and device for recovering sodium sulphide wastewater in barium sulphate production |
| 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 |
| CN104971597A (en) * | 2014-04-10 | 2015-10-14 | 中国石油化工股份有限公司 | Technical method and device of producing sodium hydrosulfide from acid gas |
| CN104971597B (en) * | 2014-04-10 | 2017-06-20 | 中国石油化工股份有限公司 | A kind of sour gas produces NaHS process and device |
| CN104370783A (en) * | 2014-10-30 | 2015-02-25 | 天津河清化学工业有限公司 | Hydrogen sulfide recycling method and hydrogen sulfide recycling system for continuously producing mercaptoacetic acid by adopting sodium hydrosulfide method |
| CN106744710A (en) * | 2017-01-20 | 2017-05-31 | 山东金典化工有限公司 | The method that continuity method produces NaHS |
| CN106744710B (en) * | 2017-01-20 | 2021-02-19 | 山东金典化工有限公司 | Method for producing sodium hydrosulfide by continuous process |
| CN115212706A (en) * | 2022-07-11 | 2022-10-21 | 江苏楷鼎环保装备有限公司 | Tail gas treatment method for sulfur black dye production system |
| CN115212706B (en) * | 2022-07-11 | 2023-08-18 | 江苏楷鼎环保装备有限公司 | Tail gas treatment method for sulfur black dye production system |
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Application publication date: 20121107 |