CN106145058A - Saturated hydrog en sulphide solution safely prepare apparatus and method - Google Patents
Saturated hydrog en sulphide solution safely prepare apparatus and method Download PDFInfo
- Publication number
- CN106145058A CN106145058A CN201510130207.5A CN201510130207A CN106145058A CN 106145058 A CN106145058 A CN 106145058A CN 201510130207 A CN201510130207 A CN 201510130207A CN 106145058 A CN106145058 A CN 106145058A
- Authority
- CN
- China
- Prior art keywords
- bottle
- separatory funnel
- saturated
- suction
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a kind of saturated hydrog en sulphide solution safely prepares device and method, including: it is sequentially connected with separatory funnel, bottle,suction, Drexel bottle, lead acetate instruction device, exhaust gas processing device, spherical air pump.Wherein, separatory funnel is provided with acid adding piston, and the bottom of separatory funnel is stretched in bottle,suction, and makes acid adding piston be maintained at the outside of bottle,suction；Ball-type extraction valve includes three gateways, and one of them gateway connects exhaust gas processing device, and two other gateway is respectively water inlet and outlet, and water inlet is provided with water valve.Opening water valve, spherical air pump starts to bleed, and slowly opens acid adding piston, the H in bulb shape separatory funnel2SO4Solution joins splendid attire Na2In the bottle,suction of S reagent.The H produced2S gas is pumped down in Drexel bottle, by distilled water solution absorption therein；Unabsorbable H2S gas can stop through lead acetate cotton blackening, reaction.Tail gas enters exhaust gas processing device, prepared by saturated solution.
Description
Technical field
The present invention relates to coal chemical technology, more particularly, it relates to the safety of saturated hydrog en sulphide solution
Preparation facilities and method.
Background technology
In ammonium sulfate standard (GB535-1995) during heavy metal (in terms of the Pb) assay of ammonium sulfate
Saturated H need to be used2S aqueous solution, but without concrete preparation process.H in textbook2S gas prepares warp
Allusion quotation method is to use kipp gas generator or the easy device of gas processed: FeS is put into kipp gas generator
In spheroplast, in funnel, inject dilute HCl.H need to be used2During S, opening airway piston, FeS is with dilute
HCl contact produces H2S, during stopping gas, only needs closure piston reaction to stop.Kipp gas generator
Mainly solve H2Problem prepared by S gas, but H2How S gas collects (dissolve or absorb), as
What judges saturated, H2The excessive security problems that affects of S gas can not solve.
Chinese patent CN200910102546 discloses and produces precipitated calcium carbonate coproduction sulfur with crude calcium sulfide
The method changing hydrogen, uses crude calcium sulfide saturated hydrogen sulphide solution dissolution after grinding, obtains sulfur under room temperature
Calcium hydride solution.Clear liquid is passed through CO2Gas, generates precipitated calcium carbonate precipitation, the not raw sulfuration of pregnancy ceased
Hydrogen, a hydrogen sulfide gas part for generation is used for being passed through filtrate and produces saturated hydrogen sulphide solution, returns
Returning upper operation dissolution crude calcium sulfide to recycle, remaining cabinet of supplying gas stores.The saturated sulfur that this invention produces
Change hydrogen and contain more Ca2+、CO3 2-Deng impurity, and the most saturated being difficult to is judged.
Hydrogen sulfide (H2S) aqueous solution, hydrosulphuric acid, is a kind of weak acid.The 1 volume of water energy when 20 DEG C
Dissolve the H of 2.6 volumes2S, concentration is about 0.1mol/L.H2S is a kind of acute severe toxicity, sucks few
Amount high concentration H2S can be fatal within the short time.H2S is to have zest and asphyxiant colourless gas.
Low concentration contact only has respiratory tract and the local irritant effect of eye, and during high concentration, general action is more apparent,
Show as central nervous system symptom and symptom of suffocating.Operating worker poisoning is not uncommon for.
The saturated H of the most existing one2S aqueous solution preparation facilities, the saturated H of this device2S
Aqueous solution preparation flow is:
After device is connected by figure, opening water valve, air pump 4 starts to bleed, in reaction bulb 1
Add a certain amount of Na2S reagent, drips H from adding entrance 22SO4Solution and Na2S reacts generation
H2S gas, H2S gas is pumped down to, equipped with in the absorption bottle 3 of distilled water, be dissolved in wherein, until
Solution turned cloudy can stop dripping H2SO4, saturated H2S aqueous solution is prepared complete.
In use finding, said apparatus exists following the most not enough:
2.1 from H2SO4Solution adds entrance and there is a large amount of H in spherical air pump exit2S gas overflowing,
Although reacting in fume hood, but equally exist potential safety hazard；
Distilled water in 2.2 absorption bottles becomes cloudy after reaction starts soon, prolongation over time
More and more muddy, but cannot judge when the distilled water in absorption bottle can dissolve abundant H2S gas
Body also reaches degree of saturation, it is therefore desirable to consume more H2SO4Solution and Na2S reagent.
Inquiry related data, has no other saturated H2Apparatus and method prepared by S aqueous solution.
Summary of the invention
For the deficiencies in the prior art, it is an object of the invention to provide saturated hydrog en sulphide solution
Safely prepare apparatus and method.
For achieving the above object, the present invention adopts the following technical scheme that
A kind of saturated hydrog en sulphide solution safely prepare device, including separatory funnel, acid adding piston,
Bottle,suction, Drexel bottle, lead acetate instruction device, exhaust gas processing device, spherical air pump, water valve.
Separatory funnel is provided with acid adding piston, and the bottom of separatory funnel is stretched in bottle,suction, and makes acid adding piston
Being maintained at the outside of bottle,suction, bottle,suction is sequentially connected with at Drexel bottle, lead acetate instruction device, tail gas
Reason device, ball-type extraction valve includes three gateways, and one of them gateway connects exhaust gas processing device,
Two other gateway is respectively water inlet and outlet, and water inlet is provided with water valve.
According to one embodiment of the invention, separatory funnel is bulb shape separatory funnel.
According to containing H in one embodiment of the invention, bulb shape separatory funnel2SO4Solution, in bottle,suction
Contain Na2S reagent.
According to one embodiment of the invention, H2SO4Solution concentration is 40%～70% (V/V).
For achieving the above object, the present invention also adopts the following technical scheme that
A kind of safe preparation method of saturated hydrog en sulphide solution, including: be sequentially connected with separatory funnel,
Bottle,suction, Drexel bottle, lead acetate instruction device, exhaust gas processing device, spherical air pump；Wherein,
Separatory funnel is provided with acid adding piston, and the bottom of separatory funnel is stretched in bottle,suction, and makes acid adding piston
It is maintained at the outside of bottle,suction；Ball-type extraction valve includes three gateways, and one of them gateway connects
Exhaust gas processing device, two other gateway is respectively water inlet and outlet, and water inlet is provided with water
Valve；Opening water valve, spherical air pump starts to bleed, and slowly opens acid adding piston, bulb shape separatory funnel
In H2SO4Solution joins splendid attire Na2In the bottle,suction of S reagent.The H produced2S gas is taken out
To Drexel bottle, by distilled water solution absorption therein；Unabsorbable H2S gas is through lead acetate
Cotton instruction device, when the complete blackening of lead acetate Cotton Gossypii produces PbS black precipitate, represents that reaction can stop
Only.Tail gas enter exhaust gas processing device, therein the most undissolved and with lead acetate [Pb (CH3COO)2]
The H of reaction2S gas is absorbed by the solution chemistry dissolved with NaOH.Saturated H2Prepared by S aqueous solution.
This device uses in being put in fume hood, uses H2Whether S gas alarm instrument has H to device2S gas is excessive
Check.
According to one embodiment of the invention, separatory funnel is bulb shape separatory funnel.
According to containing H in one embodiment of the invention, bulb shape separatory funnel2SO4Solution, in bottle,suction
Contain Na2S reagent.
According to one embodiment of the invention, H2SO4Solution concentration is 40%～70% (V/V).
In technique scheme, the saturated hydrog en sulphide solution of the present invention safely prepare device and side
Method need to be used when aiming to solve the problem that heavy metal (in terms of the Pb) assay of ammonium sulfate (GB535-1995)
Saturated H2The making of S aqueous solution reagent, and have saturated H2The terminal whether S aqueous solution has been prepared refers to
Show, improve H2The safety of the making of S aqueous solution, eliminates H2The S harm to the personnel of analysis.
Accompanying drawing explanation
Fig. 1 is the structural representation of the preparation facilities of existing hydrogen sulfide solution；
Fig. 2 is the structural representation safely preparing device of saturated hydrog en sulphide solution of the present invention.
Detailed description of the invention
Technical scheme is further illustrated below in conjunction with the accompanying drawings with embodiment.
What the present invention disclosed a kind of saturated hydrog en sulphide solution safely prepares device and preparation method thereof, root
According to H2The character of S, utilizes common glass apparatus to be assembled into a kind of reaction-absorption-instruction-vent gas treatment
Device, as shown in Figure 2: successively by bulb shape separatory funnel 5, acid adding piston 6, bottle,suction 7, wash
Gas cylinder 8, lead acetate instruction device 9, exhaust gas processing device 10, spherical air pump 11, water valve 12
Etc. being formed by connecting, and it is furnished with hydrogen sulfide alarm.
As in figure 2 it is shown, separatory funnel 5 is provided with acid adding piston 6, the bottom of separatory funnel 5 is stretched into
In bottle,suction 7, and making acid adding piston 6 be maintained at the outside of bottle,suction 7, bottle,suction 7 is sequentially connected with
Drexel bottle 8, lead acetate instruction device 9, exhaust gas processing device 10.Ball-type extraction valve 11 includes three
Gateway, one of them gateway connect exhaust gas processing device 10, two other gateway be respectively into
The mouth of a river and outlet, water inlet is provided with water valve 12.
Additionally, the safe preparation method of the saturated hydrog en sulphide solution of the present invention is:
Opening water valve 12, spherical air pump 11 starts to bleed, and slowly opens acid adding piston 6, spherical
H in separatory funnel 52SO4Solution joins splendid attire Na2In the bottle,suction 7 of S reagent.
The present invention selects H2SO4Mainly volatility is little, H2SO4Concentration is 40%～70% (V/V),
Preferably 50% (V/V).H2SO4As the highest, easily there is oxidation-reduction reaction, concentration in concentration
The lowest can dissolve H2S。
Na in bottle,suction 72S reagent also can replace with reagent such as chemical pure FeS, the H of generation2S
Gas is pumped down in Drexel bottle 8, by distilled water solution absorption therein, it is impossible to absorbed H2S gas
Body indicates device 9 through lead acetate cotton, when the complete blackening of lead acetate Cotton Gossypii produces PbS black precipitate, table
Show that reaction can stop.
Tail gas enters exhaust gas processing device 10, therein the most undissolved and and lead acetate
[Pb(CH3COO)2] H that reacts2S gas is absorbed by the solution chemistry dissolved with NaOH.Vent gas treatment
NaOH solution in device can be with repeatedly, until changing less than 10 with PH reagent paper test pH value again.
Now, saturated H2Prepared by S aqueous solution.Assembly of the invention uses in should being put in fume hood,
Use H2Whether S gas alarm instrument has H to device2S gas is excessive to be checked.
The reaction principle of the inventive method is:
H2S gas reaction of formation: H2SO4+Na2S→Na2SO4+H2S↑
Side reaction: such as H2SO4During excess, 3H2SO4+H2S→4SO2↑+4H2O
H2During S excess: 3H2S+H2SO4→4H2O+3S↓
H2S and dense H2SO4When concentration difference is few: H2S+H2SO4=S ↓+SO2↑+2H2O
H2S gas examination reacts: Pb (CH3COO)2+H2S→PbS↓+2CH3COOH
H2S aerochemistry absorbs reaction: H2S+2NaOH→Na2S+2H2O
During NaOH deficiency: H2S+Na2S→2NaHS
Continue the function of liquid feeding owing to separatory funnel is existing, have again the effect playing water seal simultaneously, solve
Original device adds H2SO4H at solution2The potential safety hazard that S gas is excessive；Contain at the tail gas of alkali liquor
Reason device can fully absorb the H being not dissolved in distilled water2S gas, solves air pump exit
H2The potential safety hazard that S gas is excessive；Lead acetate [Pb (CH3COO)2] same to H2S reaction generates black
PbS, can be as saturated H2The End point indication device whether S aqueous solution has been prepared, which solves
The problem that cannot judge to react end opportunity.
Assembly of the invention and method is further illustrated below by several embodiments.
A kind of saturated hydrog en sulphide solution safely prepare device: by bulb shape separatory funnel 5, acid adding piston
6, bottle,suction 7, Drexel bottle 8, lead acetate instruction device 9, exhaust gas processing device 10, spherical bleed
Pump 11, water valve 12 etc. are sequentially connected with, and join a hydrogen sulfide alarm.
Embodiment 1
100mL bulb shape separatory funnel built-in 40% (V/V) H2SO4Solution；Bottle,suction is built with change
Learn pure Na2S reagent；Drexel bottle is built with distilled water, in order to H2S GAS ABSORPTION；Lead acetate indicates
Being filled with lead acetate in device cotton, lead acetate cotton is being ventilated after being soaked in 10% lead acetate solution by Cotton Gossypii
Dry in cupboard and make；Exhaust gas processing device is built with 10%NaOH solution.
Saturated hydrog en sulphide solution preparation method: connect each device by Fig. 2, opens water valve 12, ball
Shape air pump 11 starts to bleed, and slowly opens acid adding piston 6, the dense H in bulb shape separatory funnel 52SO4
Join splendid attire Na2In the bottle,suction 7 of S, the H of generation2S gas is pumped down in Drexel bottle 8, no
Can absorbed H2S gas enters exhaust gas processing device 10 after lead acetate instruction device 9, works as acetic acid
The cotton blackening completely of lead, represents that reaction can stop, saturated H2Prepared by S aqueous solution.This device is put
Use in fume hood, a H by device, can be placed2S gas alarm instrument determines whether H2S gas
Excessive.Must change after the cotton use every time of lead acetate, the 10%NaOH solution in exhaust gas processing device is used
Rear in waste liquid barrel.
Embodiment 2
250mL bulb shape separatory funnel built-in 70% (V/V) H2SO4Solution；Bottle,suction is built with change
Learn pure FeS reagent；Drexel bottle is built with distilled water, in order to H2S GAS ABSORPTION；Lead acetate instruction dress
Be filled with lead acetate in putting cotton, lead acetate cotton soaked in 20% lead acetate solution by Cotton Gossypii after at fume hood
Inside dry and make；Exhaust gas processing device built with 20% NaOH solution.
Saturated hydrog en sulphide solution preparation method: connect each device by Fig. 2, opens water valve 12, ball
Shape air pump 11 starts to bleed, and slowly opens acid adding piston 6, the dense H in bulb shape separatory funnel 52SO4
Join in the bottle,suction 7 containing FeS, the H of generation2S gas is pumped down in Drexel bottle 8, it is impossible to
Absorbed H2S gas enters exhaust gas processing device 10 after lead acetate instruction device 9, works as lead acetate
Cotton blackening completely, represents that reaction can stop, saturated H2Prepared by S aqueous solution.This device is put in
Use in fume hood, a H by device, can be placed2S gas alarm instrument determines whether H2Outside S gas
Overflow.Must change after the cotton use every time of lead acetate, the NaOH solution of 20% in exhaust gas processing device is used
Rear test pH value is 14, can be continuing with in next time.
Through overtesting, never there is H in apparatus and method of the present invention2S is excessive or gas alarm instrument report
Alert situation occurs.Because of End point indication, H2The preparation time of S saturated aqueous solution is the most steady
It is scheduled on about 5min.This apparatus structure is reasonable, easy-to-operate, and End point indication is clear and definite, prepares
The H come2S saturated aqueous solution disclosure satisfy that the requirement of heavy metal (in terms of Pb) assay, and
Eliminate H in preparation process2The potential safety hazard that S gas is excessive.
Those of ordinary skill in the art is it should be appreciated that above embodiment is intended merely to
The bright present invention, and it is not used as limitation of the invention, as long as at the spirit of the present invention
In, change, the modification of embodiment described above all will be fallen in the range of claims of the present invention.
Claims (8)
1. a saturated hydrog en sulphide solution safely prepare device, it is characterised in that including:
Separatory funnel, acid adding piston, bottle,suction, Drexel bottle, lead acetate instruction device, vent gas treatment
Device, spherical air pump, water valve；
Described separatory funnel is provided with described acid adding piston, and described bottle,suction is stretched in the bottom of separatory funnel
In, and make described acid adding piston be maintained at the outside of described bottle,suction；
Described bottle,suction is sequentially connected with described Drexel bottle, lead acetate instruction device, exhaust gas processing device；
Described ball-type extraction valve includes three gateways, and one of them gateway connects described vent gas treatment
Device, two other gateway is respectively water inlet and outlet, and described water inlet is provided with described water
Valve.
2. saturated hydrog en sulphide solution as claimed in claim 1 safely prepare device, its feature exists
In, described separatory funnel is bulb shape separatory funnel.
3. saturated hydrog en sulphide solution as claimed in claim 2 safely prepare device, its feature exists
In, contain H in described bulb shape separatory funnel2SO4Solution, contains Na in described bottle,suction2S reagent.
4. saturated hydrog en sulphide solution as claimed in claim 3 safely prepare device, its feature exists
In, described H2SO4Solution concentration is 40%～70% (V/V).
5. the safe preparation method of a saturated hydrog en sulphide solution, it is characterised in that including:
It is sequentially connected with separatory funnel, bottle,suction, Drexel bottle, lead acetate instruction device, vent gas treatment dress
Put, spherical air pump；
Wherein, described separatory funnel is provided with acid adding piston, and described sucking filtration is stretched in the bottom of separatory funnel
In Ping, and described acid adding piston is made to be maintained at the outside of described bottle,suction；
Described ball-type extraction valve includes three gateways, and one of them gateway connects described vent gas treatment
Device, two other gateway is respectively water inlet and outlet, and described water inlet is provided with described water
Valve；
Opening water valve, spherical air pump starts to bleed, and slowly opens acid adding piston.
6. the safe preparation method of saturated hydrog en sulphide solution as claimed in claim 5, its feature exists
In, described separatory funnel is bulb shape separatory funnel.
7. the safe preparation method of saturated hydrog en sulphide solution as claimed in claim 6, its feature exists
In, contain H in described bulb shape separatory funnel2SO4Solution, contains Na in described bottle,suction2S reagent.
8. the safe preparation method of saturated hydrog en sulphide solution as claimed in claim 7, its feature exists
In, described H2SO4Solution concentration is 40%～70% (V/V).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510130207.5A CN106145058A (en) | 2015-03-24 | 2015-03-24 | Saturated hydrog en sulphide solution safely prepare apparatus and method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510130207.5A CN106145058A (en) | 2015-03-24 | 2015-03-24 | Saturated hydrog en sulphide solution safely prepare apparatus and method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106145058A true CN106145058A (en) | 2016-11-23 |
Family
ID=58063981
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510130207.5A Pending CN106145058A (en) | 2015-03-24 | 2015-03-24 | Saturated hydrog en sulphide solution safely prepare apparatus and method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106145058A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112938905A (en) * | 2021-04-23 | 2021-06-11 | 中国科学院过程工程研究所 | Method for preparing high-purity sulfur by using tail gas containing hydrogen sulfide |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102041994A (en) * | 2010-11-12 | 2011-05-04 | 上海科油石油仪器制造有限公司 | Hydrogen sulfide early-warning measuring method |
-
2015
- 2015-03-24 CN CN201510130207.5A patent/CN106145058A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102041994A (en) * | 2010-11-12 | 2011-05-04 | 上海科油石油仪器制造有限公司 | Hydrogen sulfide early-warning measuring method |
Non-Patent Citations (3)
| Title |
|---|
| 廖仕孟等: "《天然气采输作业硫化氢防护》", 28 February 2013, 重庆大学出版社 * |
| 李祥福: "介绍一种制取硫化氢及其饱和溶液的装置", 《中国医院药学杂志》 * |
| 钟伦恒: "再介绍一种简易硫化氢发生装置", 《中国医院药学杂志》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112938905A (en) * | 2021-04-23 | 2021-06-11 | 中国科学院过程工程研究所 | Method for preparing high-purity sulfur by using tail gas containing hydrogen sulfide |
| CN112938905B (en) * | 2021-04-23 | 2023-05-30 | 中国科学院过程工程研究所 | Method for preparing high-purity sulfur by utilizing tail gas containing hydrogen sulfide |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103691274B (en) | A kind of method of producing regulation and control for Complexing Iron sulfur removal technology | |
| CN108211749B (en) | Wet desulfurization spray tower and desulfurization method | |
| CN201147664Y (en) | Whole set processing equipment for hydrogenchloride and sulfuric dioxide tail gas | |
| CN106145058A (en) | Saturated hydrog en sulphide solution safely prepare apparatus and method | |
| CN104028083B (en) | A kind of fluorinated tail gas treating apparatus and method | |
| CN203447970U (en) | Acid mist absorbing and recycling system | |
| CN205760554U (en) | A kind of chloride exhaust gas processing device | |
| CN104816874A (en) | Medicine sealing device capable of automatically controlling opening and closing and sealing method | |
| CN103550989B (en) | The integrated conduct method of tail gas in a kind of mercury chloride production process | |
| CN109157964A (en) | A kind of viscose rayon waste gas absorbing system and method | |
| CN204237560U (en) | A kind of device preparing Sodium sulfhydrate | |
| CN107126828A (en) | A kind of method of comprehensive utilization of solution of gold smelting plant relieving haperacidity flue gas | |
| CN110194439A (en) | The system and method for spray combustion sulphur-furnace production purifying sulfur dioxide | |
| CN104857827A (en) | Fuming sulfuric acid neutralization treatment apparatus and fuming sulfuric acid neutralization treatment process for sulfonation production | |
| CN203469786U (en) | Respiratory gas processing device applicable to titanium tetrachloride production process | |
| CN209123641U (en) | A kind of electron level Waste Sulfuric Acid processing mechanism with hydrogen peroxide | |
| CN206751389U (en) | A kind of chlorine recovery system during pyridine compounds and their continuous chlorination | |
| CN109045983A (en) | A kind of stable operation minimum discharge ammonia desulfuration equipment | |
| CN205598939U (en) | Automatic change desulphurization of exhaust gas system | |
| CN101343038A (en) | Recovery method for mix waste gas of hydrogen chloride and sulphur dioxide in lipoic acid preparation | |
| CN209612594U (en) | High purity acid synthesizer exhaust treatment system | |
| CN205627584U (en) | Nitrate water dealkalize flue gas desulfurization jar | |
| CN104587810B (en) | A kind of method of comprehensive utilization of the chlorination tail gas of itrated compound | |
| CN208599454U (en) | The system of hydrogen sulfide tail gas processing in a kind of tungsten smelting process | |
| CN110229934A (en) | New and effective sulfurous method sugar refining technology |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20161123 |
|
| RJ01 | Rejection of invention patent application after publication |