CN1075299A - Process for purifying of sodium sulfide - Google Patents
Process for purifying of sodium sulfide Download PDFInfo
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- CN1075299A CN1075299A CN 92114398 CN92114398A CN1075299A CN 1075299 A CN1075299 A CN 1075299A CN 92114398 CN92114398 CN 92114398 CN 92114398 A CN92114398 A CN 92114398A CN 1075299 A CN1075299 A CN 1075299A
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Abstract
The present invention relates to the production technique of sodium sulphite, it is a kind of process for purifying of sodium sulfide, its technology is as follows: coal and thenardite mixing back roasting are generated thick alkali, cooling leaching obtains high alkali liquid first then, and its characteristics are every cubic metre of iron removing reagent that adds 4 to 8 kilograms first in the high alkali liquid, and alkali liquid temperature is controlled at 50 ℃ to 100 ℃, the best is 65 ℃ to 85 ℃, after stirring, the settling time is no less than 4 hours, carries out solid-liquid separation again and obtains once refining alkali lye; Its technology is simple, and environmental pollution is few, and the finished product not only content of iron is low, and foreign matter content such as yellow soda ash, sodium-chlor, Sulfothiorine, S-WAT is also lower.
Description
The present invention relates to the production technique of sodium sulphite, is a kind of process for purifying of sodium sulfide.
Producing high-purity technical sodium sulphite at present has the method for employing caustic soda soln absorbing hydrogen sulphide gas to obtain, and as the P P G company of the U.S., adopts and produces CS
2The byproduct hydrogen sulfide produce high-purity technical sodium sulphite, its equation is:
But the cost of this method is higher, and output is restricted, and should not carry out large-scale industrial production.
Adopt the production technique of coal reduction thenardite to produce sodium sulphite in addition, its equation is:
Feed coal and thenardite are mixed the back by a certain percentage to add converter or open hearth and carries out roasting generate thick alkali under 800 ℃ to 1100 ℃, leach with the aqueous solution when being cooled to 400 ℃ to 700 ℃ then and carry out heat of solution, the high alkali liquid of leaching obtains finished product after sending evaporization process evaporation concentration packing after the clarification, and in the leaching operation isolated solid slag after washing the sodium sulphite of bricklayer's preface with water dissolution remnants, again through solid-liquid separation, isolated sig water is returned the leaching operation be used for leaching, body refuse is discharged from transports to specified slag field; Because of containing impurity such as iron, yellow soda ash in feed coal and the thenardite, and equipment all is made of iron, make the content of impurity such as iron in the finished product, yellow soda ash higher, thereby can't satisfy the high requirement of fine chemistry industry industry, the technical process Fig. 1 in its technical process such as the accompanying drawing the sodium sulphite quality.
The objective of the invention is to propose a kind of industrial sodium sulfide process for refining.Its measure is following: this industrial sodium sulfide process for refining is that coal and thenardite mixing back roasting are generated thick alkali, the cooling leaching obtains high alkali liquid first then, be characterized in the iron removing reagent that adds 4 to 8 kilograms first in the high alkali liquid at every cubic metre, alkali liquid temperature is controlled at 50 ℃ to 100 ℃, the best is 65 ℃ to 85 ℃, after stirring, settling time is no less than 4 hours, carry out solid-liquid separation again and obtain hanging down the once refining alkali lye of iron-holder, its iron removing reagent can be zinc oxide, activated alumina, Manganse Dioxide, calcium oxide, tertiary sodium phosphate; Wash the mud of bricklayer's preface with once making with extra care after the remaining solid slag in back is put into the leaching operation,, thereby reduce pollution environment so that reclaim the sodium sulphite in the solid slag; In order further to remove once impurity such as yellow soda ash in the smart alkali lye, sodium-chlor, Sulfothiorine, S-WAT, to once make with extra care alkali lye at 20 ℃ to 45 ℃, the best is to carry out crystallization under 25 ℃ to 35 ℃, and solid-liquid separation is obtained the crystalline sodium sulfide of secondary refining, and being returned, the isolated mother liquor of secondary refining makes full use of in the leaching liquid of thick alkali leaching operation, minimizing is to the pollution of environment, and leaching temperature promptly first the high alkali liquid temperature be controlled at more than 80 ℃, the best is 90 ℃; To once make with extra care alkali lye or crystalline sodium sulphite dissolves under 100 ℃ at 50 ℃, the best is 70 ℃ to 90 ℃, be placed on vacuum tightness and be 0.06MPa to 0.07MPa, temperature and be in 150 ℃ to 160 ℃ the vaporizer after the evaporation concentration (also can adopt atmospheric evaporation), again barrelling or to obtain not only iron-holder through packaging means such as pelleter film-makings low but also contain the high-purity technical sodium sulphite finished product of the low different grades of impurity level such as yellow soda ash; In order to reduce bringing into of ferrous contaminants in the technological process, from the once container of the alkali lye process of refining beginning or container or the equipment that equipment surface is non-iron.The technical process of the embodiment of the invention such as the technical process Fig. 2 in the accompanying drawing.
The invention will be further described below in conjunction with embodiment and technical process:
Embodiment 1:
Coal and thenardite are generated thick alkali by carrying out roasting in 20: 100 to 25: 100 the weight percent mixing back adding converter under 800 ℃ to 1100 ℃, when being cooled to 400 ℃ to 700 ℃ then, leach and promptly carry out thermosol and solid-liquid is separated with the aqueous solution, its separate mode adopts sedimentation clarification back to separate, obtaining Containing Sulfur sodium is the high alkali liquid first of 20～30% weight percents, and leaching temperature promptly first the high alkali liquid temperature be controlled at more than 80 ℃, the best is 90 ℃; It is the container of non-iron that high alkali liquid is first put into the surface, then at every cubic metre of iron removing reagent that adds 4 to 8 kilograms first in the high alkali liquid, iron removing reagent is preferably activated alumina, add-on is 4 kilograms/every cubic metre high alkali liquid first, also can be: zinc oxide, add-on are 5 kilograms/every cubic metre high alkali liquid first; Manganse Dioxide, add-on are 8 kilograms/every cubic metre high alkali liquid first; Calcium oxide, add-on are 7 kilograms/every cubic metre high alkali liquid first; Tertiary sodium phosphate, 6 kilograms/every cubic metre high alkali liquid first; Alkali liquid temperature is controlled at 50 ℃ to 100 ℃, the best is 65 ℃ to 85 ℃, after stirring, settling time is no less than 4 hours, the best is 6 hours, carries out solid-liquid separation again and obtains once refining alkali lye, and its separate mode adopts filter method: will once make with extra care the remaining solid slag in back and put into and leach the mud of washing bricklayer's preface after the operation, so that the sodium sulphite in the recovery filter residue, thereby minimizing is to the pollution of environment; If only need the lower sodium sulphite of iron-holder, can be to reduce to normal temperature in the atmospheric evaporation container of non-iron after the evaporation concentration and be packaged to be the industrial sodium sulfide finished product that hangs down iron-holder for the bucket of non-iron through the surface with refining alkali lye once with the surface.Result's following [by weight percentage] after tested: to contain the Fe amount be 0.0046% to high alkali liquid first, and it is 0.0023% that once refining alkali lye contains the Fe amount, and the deironing rate is 50.0%.
The yellow soda ash that still contains part in the sodium sulphite because of smart alkali lye gained once, sodium-chlor, Sulfothiorine, impurity such as S-WAT, such product can't satisfy some special service requirements of fine chemistry industry industry, can remove above-mentioned impurity by the crystallization control temperature, its method is as follows: will once make with extra care alkali lye at 20 ℃ to 45 ℃, the best is 25 ℃ and carries out crystallization to 35 ℃ of lower surfaces container that is non-iron, best Tc is 30 ℃, and solid-liquid separation is obtained the crystalline sodium sulfide of secondary refining, its separate mode can be used centrifugal separation method, make full use of in the leaching liquid of thick alkali leaching operation and the isolated mother liquor of secondary refining is returned, reduce pollution environment; Result's following (by weight percentage) after tested: high alkali liquid first, Containing Sulfur sodium 24.5% contains yellow soda ash 2.5%, and iron-holder is 0.0046%; Secondary refining alkali lye, Containing Sulfur sodium 30.4% contains yellow soda ash 0.42%, and iron-holder is 0.0008%.
To once make with extra care alkali lye or crystalline sodium sulphite dissolves under 100 ℃ at 50 ℃, the best is 70 ℃ to 90 ℃, the surface that is placed on vacuum tightness and is 0.06MPa, temperature and be 155 ℃ is in the vaporizer of non-iron after the evaporation concentration, and it is low but also contain the high-purity technical sodium sulphite finished product of the low different grades of impurity level such as yellow soda ash through the surface to be that the pelleter film-making packaging means of non-iron obtains not only iron-holder again.Basic identical in other operation of this embodiment and the existing technical process.
Embodiment 2:
Containing Sulfur sodium is 25% 150 cubic metres high alkali liquids first, in the surface is the container of titanium system, be controlled under 70 ℃ in temperature, add 1160 kilograms of iron removing reagent activated aluminas, after stirring, sedimentation 5 hours, separate mode obtains 134 cubic metres of once refining alkali lye with solid-liquid separation after filtration, result's following [by weight percentage] after tested: the high alkali liquid iron-holder is 0.0050% first, and once refining alkali lye iron-holder is 0.0029%, and the deironing rate is 42.0%; On the surface is the container of titanium system, be controlled under 27 ℃ in temperature, carry out crystallization, utilize crystalline sodium sulfide that the centrifugation mode obtains secondary refining with solid-liquid separation result's following (by weight percentage) after tested then: high alkali liquid first, Containing Sulfur sodium 21.5%, contain yellow soda ash 3.0%, iron-holder is 0.0050%; Secondary refining alkali lye, Containing Sulfur sodium 25.4% contains yellow soda ash 0.45%, and iron-holder is 0.0009%.And mother liquor returns the leaching operation for 84 cubic metres, and with leaching temperature promptly first the high alkali liquid temperature be controlled at 85 ℃, utilize the principle of saltouing to make after the impurity crystallization such as yellow soda ash to be discharged to and wash bricklayer's preface with solid slag; Under 80 ℃, the crystalline sodium sulfide of secondary refining dissolved and obtain 63.5 cubic metres of secondary refining alkali lye, send into again in the vaporizer of nickel system, in vacuum tightness is that 0.06MPa, temperature are under 160 ℃, after the evaporation concentration, it is low but also contain 25.025 tons of low high-purity technical sodium sulphite finished products of impurity level such as yellow soda ash through the surface to be that the pelleter film-making packaging means of manganese system obtains not only iron-holder again.Basic identical in other operation of this embodiment and embodiment 1 and the existing technical process.(100%) 1574 kilogram of embodiment 2 actual ton consumption raw material thenardite, (100%) 374 kilogram of coal dust.
Technology of the present invention is simple, cost is low, environmental pollution is few, with this explained hereafter gained high-purity technical sodium sulphite product, not only the content of iron is low, and foreign matter content such as yellow soda ash, sodium-chlor, Sulfothiorine, S-WAT is also lower, and is near or below domestic or international standard, and its contrast is as follows:
| Project | The Japan U.S. | The new BOO14-89 acceptable end product of Chinese Enterprise standard | Embodiment 1 | Embodiment 2 | |||
| Reach Cao Da Co., Ltd. | Three field buttocks KCCs | Vinch Limi | Emjcal Teal | ||||
| Total reduzate Na 2S%≥ | 60.0 | 60.0 | 60.0 | 60.0 | |||
| Na 2S%≥ | 58.0 | 58.0 | 60.0 | 62.26 | 62.85 | ||
| Na 2CO 3%≤ | 1.5 | 1.5 | 2.0 | 1.5 | 1.09 | 1.07 | |
| Na 2SO 3%≤ | 1.0 | 1.0 | 2.0 | 0.18 | 0.1 | ||
| Na 2S 2O 3%≤ | 1.0 | 1.0 | 4 | 1.0 | 2.0 | 0.91 | 0.48 |
| Iron (Fe) ‰≤ | 0.04 | 0.06 | 0.005 | 0.012 | 0.03 | 0.021 | 0.021 |
Claims (8)
1, a kind of process for purifying of sodium sulfide, coal and thenardite mixing back roasting are generated thick alkali, the cooling leaching obtains high alkali liquid first then, it is characterized in that every cubic metre of iron removing reagent that adds 4 to 8 kilograms first in the high alkali liquid, alkali liquid temperature is controlled at 50 ℃ to 100 ℃, and the best is 65 ℃ to 85 ℃, after stirring, settling time is no less than 4 hours, carries out solid-liquid separation again and obtains once refining alkali lye.
2, process for purifying of sodium sulfide according to claim 1 is characterized in that iron removing reagent can be zinc oxide, activated alumina, Manganse Dioxide, calcium oxide, tertiary sodium phosphate.
3, process for purifying of sodium sulfide according to claim 1 is characterized in that the remaining solid slag in refining back is once put into the mud of washing bricklayer's preface after the leaching operation.
4, process for purifying of sodium sulfide according to claim 1 is characterized in that and will once make with extra care alkali lye at 20 ℃ to 45 ℃ that the best is under 25 ℃ to 35 ℃, carries out crystallization, and solid-liquid separation is obtained the crystalline sodium sulfide of secondary refining.
5, process for purifying of sodium sulfide according to claim 4 is characterized in that the isolated mother liquor of secondary refining is returned in the leaching liquid of thick alkali leaching operation, and leaching temperature promptly first the high alkali liquid temperature be controlled at more than 80 ℃, the best is 90 ℃.
6, according to claim 1 or 4 described process for purifying of sodium sulfide, it is characterized in that once to make with extra care alkali lye or crystalline sodium sulphite dissolves under 100 ℃ at 50 ℃, the best is 70 ℃ to 90 ℃, be placed on vacuum tightness and be 0.06MPa to 0.07MPa, temperature and be in 150 ℃ to 160 ℃ the vaporizer after the evaporation concentration, again barrelling or obtain finished product through packaging means such as pelleter film-makings.
7,, it is characterized in that the container of alkali lye process or container or the equipment that equipment surface is non-iron according to claim 1 or 4 described process for purifying of sodium sulfide.
8, process for purifying of sodium sulfide according to claim 6 is characterized in that the container of alkali lye process or container or the equipment that equipment surface is non-iron.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92114398 CN1033156C (en) | 1992-12-06 | 1992-12-06 | Process for purifying of sodium sulfide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92114398 CN1033156C (en) | 1992-12-06 | 1992-12-06 | Process for purifying of sodium sulfide |
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| CN1075299A true CN1075299A (en) | 1993-08-18 |
| CN1033156C CN1033156C (en) | 1996-10-30 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 92114398 Expired - Fee Related CN1033156C (en) | 1992-12-06 | 1992-12-06 | Process for purifying of sodium sulfide |
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| CN (1) | CN1033156C (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1292981C (en) * | 2004-02-17 | 2007-01-03 | 李云政 | Process of preparing sodium sulfide from reducing sodium thiosulfate by microwave inducting carbon |
| CN1944241B (en) * | 2006-10-27 | 2010-12-29 | 自贡鸿鹤化工股份有限公司 | Process for producing high purity crystalline sodium sulfide |
| CN101353159B (en) * | 2007-07-24 | 2011-07-13 | 金贤琴 | Sodium sulfide solution purification process |
| CN106185839A (en) * | 2016-07-01 | 2016-12-07 | 深州嘉信化工有限责任公司 | A kind of production method of ultralow ferrum industrial sodium sulfide |
| CN106517101A (en) * | 2016-10-31 | 2017-03-22 | 重庆市南川区庆岩福利碱厂 | Preparation process of sodium sulfide with low content of iron |
| CN108002351A (en) * | 2016-10-31 | 2018-05-08 | 中国石油化工股份有限公司 | A kind of method of industrial goods purifying of sodium sulfide |
| CN108529571A (en) * | 2018-06-25 | 2018-09-14 | 谢秀红 | A kind of preparation method of vulcanized sodium |
| CN109455676A (en) * | 2019-01-21 | 2019-03-12 | 范冲天 | A kind of environmentally friendly refining methd of akali sulphide |
| CN114132901A (en) * | 2021-11-17 | 2022-03-04 | 重庆长能环境科技有限公司 | Method for preparing sodium sulfide from SDS desulfurization slag and product thereof |
-
1992
- 1992-12-06 CN CN 92114398 patent/CN1033156C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1292981C (en) * | 2004-02-17 | 2007-01-03 | 李云政 | Process of preparing sodium sulfide from reducing sodium thiosulfate by microwave inducting carbon |
| CN1944241B (en) * | 2006-10-27 | 2010-12-29 | 自贡鸿鹤化工股份有限公司 | Process for producing high purity crystalline sodium sulfide |
| CN101353159B (en) * | 2007-07-24 | 2011-07-13 | 金贤琴 | Sodium sulfide solution purification process |
| CN106185839A (en) * | 2016-07-01 | 2016-12-07 | 深州嘉信化工有限责任公司 | A kind of production method of ultralow ferrum industrial sodium sulfide |
| CN106517101A (en) * | 2016-10-31 | 2017-03-22 | 重庆市南川区庆岩福利碱厂 | Preparation process of sodium sulfide with low content of iron |
| CN108002351A (en) * | 2016-10-31 | 2018-05-08 | 中国石油化工股份有限公司 | A kind of method of industrial goods purifying of sodium sulfide |
| CN106517101B (en) * | 2016-10-31 | 2019-02-22 | 重庆市南川区庆岩福利碱厂 | The manufacture craft of low-iron sodium sulfide |
| CN108529571A (en) * | 2018-06-25 | 2018-09-14 | 谢秀红 | A kind of preparation method of vulcanized sodium |
| CN109455676A (en) * | 2019-01-21 | 2019-03-12 | 范冲天 | A kind of environmentally friendly refining methd of akali sulphide |
| CN109455676B (en) * | 2019-01-21 | 2022-05-27 | 范冲天 | Environment-friendly refining method of sodium sulfide |
| CN114132901A (en) * | 2021-11-17 | 2022-03-04 | 重庆长能环境科技有限公司 | Method for preparing sodium sulfide from SDS desulfurization slag and product thereof |
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| Publication number | Publication date |
|---|---|
| CN1033156C (en) | 1996-10-30 |
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