CN106185838A - Sodium sulfide preparation method - Google Patents
Sodium sulfide preparation method Download PDFInfo
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- CN106185838A CN106185838A CN201610509025.3A CN201610509025A CN106185838A CN 106185838 A CN106185838 A CN 106185838A CN 201610509025 A CN201610509025 A CN 201610509025A CN 106185838 A CN106185838 A CN 106185838A
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- sodium sulfide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/22—Alkali metal sulfides or polysulfides
- C01B17/36—Purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of sodium sulfide preparation method, comprise the following steps: S100: take and produce the sodium sulfide solution that barium sulfate produces, containing sodium sulfide 40～70g/L in this aqueous solution；S200: add 40～70g/L sodium sulfide solutions in aqueous, more than temperature 70 C, clarify more than 20 hours, filter clarification；S300: be evaporated to about 250g/L, it is thus achieved that sodium sulfide semi-finished product；S400: beaten to tramp iron separator by sodium sulfide semi-finished product, the many polyiron sulfates adding 0.1 0.3%wt make the various deposits of generation settle, stir 20 minutes temperature 70～80 DEG C of filtrations；Obtain the iron content sodium sulfide solution at below 1ppm；S500: the solution evaporation of step S400 is concentrated into 60% content, film-making i.e. obtains the iron content sodium sulfide product at below 10ppm.Sodium sulfide purity prepared by the present invention is high, and tool is widely used.
Description
Technical field
The invention belongs to chemical field, particularly to a kind of sodium sulfide preparation method.
Background technology
The industrial sodium sulfide that China produces at present has red sodium sulphide flakes, pornographic movie sodium sulfide, red sodium sulphide flakes iron content
About 300ppm, pornographic movie iron content sodium sulfide is at about 30ppm.Some particular clients are required that iron content is more lower, it is desirable to <
10ppm；Especially at copper ore dressing, sulfur dye and leather industry.As produced the senior sulfur dye of high-quality, produce softness, hands
The leather felt, improves the aspects such as leather product quality, is desirable that sodium sulfide product iron content < 10ppm.
Summary of the invention
For the defect of prior art, the invention provides a kind of sodium sulfide preparation method, comprise the following steps:
S100: take and produce the sodium sulfide solution that barium sulfate produces, in this aqueous solution containing sodium sulfide 40～
70g/L.S200: add 40～70g/L sodium sulfide solutions in aqueous, more than temperature 70 C, clarify more than 20 hours, mistake
Filter clarification.S300: be evaporated to about 250g/L, it is thus achieved that sodium sulfide semi-finished product.S400: sodium sulfide semi-finished product are beaten to tramp iron separator
In, the many polyiron sulfates adding 0.1-0.3%wt make the various deposits of generation settle, and stir 20 minutes temperature 70～80 DEG C
Filter；Obtain the iron content sodium sulfide solution at below 1ppm.S500: the solution evaporation of step S400 is concentrated into 60% content,
Film-making i.e. obtains the iron content sodium sulfide product at below 10ppm.
Optionally, also comprise the steps: S500: in solution of zinc sulfate, add manganese powder and/or manganese-base alloy powder,
Temperature is 50 DEG C and pH ＞ 4.0, stirring reaction, after react, filter separation, after through evaporating, concentrating and crystallizing, obtain high-purity
Degree zinc sulfate, adds zinc sulfate 5-10 kilogram quantities by the high-purity sulfuric acid zinc of preparation by every cube of filtrate and weighs zinc sulfate, often stand
Side's filtrate correspondence 1 cube of solution of zinc sulfate of preparation；By every cube of water adds barium sulfide 150kg, take clear liquid standby；By above two
The solution kind prepared, is simultaneously introduced in sodium sulfide filtrate, stirring, mixing speed 80 revs/min, reaction temperature control 80 DEG C with
On, then precipitation 12 16 hours, after remove impurity clarification, send evaporization process, i.e. obtain high purity sodium sulfide through evaporation and concentration.
Optionally, S600 is also comprised the steps:: take a certain amount of crystalline sodium sulfide raw material and be placed in vacuum rake dryer
In, hermetically drying machine, open vacuum pump, open roots blower. after treating that vacuum meter is stably, ON cycle oil pump, and start to add
Thermal cycle oil, controls the temperature of recycle oil, and rake type drier at the uniform velocity stirs. and after equipment runs certain time, stop stirring, close
Drying machine upper valve, is passed through nitrogen in drying machine, opens dog-house, rapid feeding, uses thermogravimetric analyzer to survey its residue
Water content. after reaction to be drained off all terminates, close vacuum pump and roots blower, stop stirring, cooling discharge；Wherein vacuum
Necessary >=0.096MPa, uses two sections of temperature to be dried, and one section of low temperature 85 DEG C carries out heating 1h；Two-stage nitration high temperature 115 DEG C is carried out
Heating 0.5h；Material is cooled to 40 DEG C with bottom discharge.
The invention has the beneficial effects as follows: production is taked stainless steel equipment such as settling tank, pipeline, pump class, vaporizer, film-making
Machines etc. avoid the introducing of iron tramp, add the spontaneous combustion sedimentation time, by adding iron removing reagent, increase defecator, more than arrange
Execute so that the iron content in sodium sulfide product is all down at below 10ppm.Use high-purity sulfuric acid zinc and barium sulfide solution, permissible
Remove the iron ion in sodium sulfide so that iron ion content is substantially reduced (less than 3ppm)；Dry run controls be dried vacuum
The conditions such as degree, baking temperature, drying time, drop temperature solve the problem that crystalline sodium sulfide is oxidizable, cohere, thus obtain
Highly purified anhydrous sodium sulfide.
Accompanying drawing explanation
Fig. 1 is the process chart of method of purification of the present invention.
Detailed description of the invention
Understandable, below in conjunction with the accompanying drawings to the present invention for enabling the above-mentioned purpose of the present invention, feature and advantage to become apparent from
Detailed description of the invention be described in detail, make above and other purpose, feature and the advantage of the present invention to become apparent from.Entirely
The part that reference instruction identical in portion's accompanying drawing is identical.Accompanying drawing the most drawn to scale, it is preferred that emphasis is illustrate this
Bright purport.
Embodiment 1
Referring to Fig. 1, the sodium sulfate purifying technique of the present invention comprises the following steps:
S100: take and produce the sodium sulfide solution that barium sulfate produces, in this aqueous solution containing sodium sulfide 40～
70g/L, alkalescence is very strong, for reducing equipment corrosion, can use stainless steel equipment pipeline pump.
S200: add 40～70g/L sodium sulfide solutions in aqueous, more than temperature 70 C, clarify more than 20 hours,
Filter clarification.Owing to producing the impurity barium that brings of barium sulfate system, iron content is higher, and adding sodium sulfide, can to remove barium etc. miscellaneous
Matter.
S300: be evaporated to about 250g/L, it is thus achieved that sodium sulfide semi-finished product；The technique that four-effect evaporation taked by evaporation equipment.
S400: beaten to tramp iron separator by sodium sulfide semi-finished product, the many polyiron sulfates adding 0.1-0.3%wt make generation
Various deposits settle, and stir 20 minutes temperature 70～80 DEG C of filtrations；Obtain the iron content sodium sulfide solution at below 1ppm.
S500: in single effect evaporator (2520 rustless steel), the solution of step S400 is concentrated into 60% content, film-making is i.e.
Obtain the iron content sodium sulfide product at below 10ppm.
In order to further remove iron ion, adding sodium carbonate, sodium hydroxide, Alumen filters precipitation and obtains filtrate
After, it is also possible to comprise the steps:
S600: preparation solution of zinc sulfate.Containing impurity elements such as more copper, cadmium, nickel, cobalts in industrial sulphuric acid zinc, if directly
Connect employing industrial sulphuric acid zinc and then can introduce impurity in the preparation of sodium sulfide.For this present invention, solution of zinc sulfate adds gold
Belonging to manganese powder and/or manganese-base alloy powder, temperature is 50 DEG C and pH ＞ 4.0, stirring reaction, after having reacted, filters and separates,
With by the copper in industrial sulphuric acid zinc, cadmium, nickel and cobalt element remove, after through evaporating, concentrating and crystallizing, i.e. obtain high-purity sulfuric acid zinc.
The reduction potential of manganese metal is higher than the reduction potential of metallic zinc, and this makes manganese metal be eager to excel the diadochy of copper, cadmium, cobalt and nickel
In metallic zinc；At a lower temperature, the deep purifying of copper, cadmium, cobalt and nickel can be realized, thoroughly change existing zinc powder and purify work
In skill, for removing copper cadmium nickel cobalt and avoiding returning of copper cadmium molten, solution need to be carried out a liter present situation for gentle cooling operation.Additionally,
The reduction potential that manganese metal is higher so that copper in purification slag, cadmium, cobalt, nickel stability are preferable, it is to avoid return the generation of molten phenomenon.
Experimental example 1
Measure 1.6L except solution of zinc sulfate after ferrum (Zn:140g/L, Cu:310mg/L, Cd:502mg/L, Ni:14.6mg/L,
Co:12.8mg/L, pH=4.9), open stirring and be heated to 50 DEG C, subsequently according to copper and 5 times of addition manganese of cadmium gross mass
Terminating reaction after copper alloy powder (Mn:98%) insulation reaction 120min, vacuum filtration also collects filtrate and filtering residue.Gained filtrate
Middle copper, cadmium, cobalt, nickel concentration be respectively 0.16,0.13,0.22,0.14mg/L, removal efficiency all more than 98%, meets impurity removal
Requirement.
The high-purity sulfuric acid zinc of preparation is added zinc sulfate 5-10 kilogram quantities by every cube of filtrate and weighs zinc sulfate, every cube
Filtrate correspondence 1 cube of solution of zinc sulfate of preparation.
Formulating vulcanization barium solution, by adding barium sulfide 150kg in every cube of water, dissolves 15Be, water by barium sulfide (BaS)
Temperature 90 DEG C, precipitates 70 minutes, takes clear liquid standby, and every cube of filtrate need to add the barium sulfide solution of 0.06-0.08 cube；More than Jiang
Two kinds of solution prepared, are simultaneously introduced in sodium sulfide filtrate, and stirring, mixing speed 80 revs/min, reaction temperature controls at 80 DEG C
Above, then precipitation 12 16 hours, in the sodium sulfide solution after remove impurity clarification, iron ion content is at 3-8PPM, then send evaporation
Operation；Through evaporation and concentration, film-making packaging, i.e. high purity sodium sulfide.
Embodiment 2
The present embodiment introduces the drying means for the high purity sodium sulfide prepared by embodiment 1.Embodiment 1 is produced
Sodium sulfide main component be Na2S·9H2O and Na2S·5.5H2O, in order to obtain anhydrous sodium sulfide, needs to be dried it
Process.
Specifically, S700: take a certain amount of crystalline sodium sulfide raw material and be placed in vacuum rake dryer, hermetically drying machine, open
Open vacuum pump, when vacuum reaches-0.08MPa in machine to be dried, open roots blower. after treating that vacuum meter is stably, unlatching follows
Ring oil pump, and begin to warm up recycle oil, controlling the temperature of recycle oil, rake type drier at the uniform velocity stirs. and equipment runs certain time
After, stop stirring, close drying machine upper valve, in drying machine, be passed through nitrogen, open dog-house, rapid feeding, use heat
Its residue water content surveyed by weight analysis instrument. and after reaction to be drained off all terminates, close vacuum pump and roots blower, stop stirring, fall
Temperature discharging.Sodium sulfide crystal to be made occurs without melted and viscous wall in process of vacuum drying, and vacuum is necessary >=0.096MPa, this
It is the crystal sodium sulfide key that can be dried production, can also effectively stop the oxidation stain of sodium sulfide simultaneously.Simultaneously
Using two sections of temperature to be dried, one section of low temperature 85 DEG C carries out heating 1h, it is to avoid fusing；Two-stage nitration high temperature 115 DEG C heats
0.5h, mainly ensures be dried completely and shorten drying time.For preventing from being dried the combustion oxidation of rear material, it is necessary to protecting
Hold under vacuum condition, material is cooled to less than 40 DEG C can discharging.
Elaborate a lot of detail in the above description so that fully understanding the present invention.But above description is only
Presently preferred embodiments of the present invention, the present invention can implement to be much different from alternate manner described here, therefore originally
Invention is not limited by disclosed above being embodied as.The most any those skilled in the art are without departing from the technology of the present invention
In the case of aspects, technical solution of the present invention is made many possible by the method and the technology contents that all may utilize the disclosure above
Variation and modification, or it is revised as the Equivalent embodiments of equivalent variations.Every content without departing from technical solution of the present invention, according to this
The technical spirit of invention, to any simple modification made for any of the above embodiments, equivalent variations and modification, all still falls within skill of the present invention
In the range of the protection of art scheme.
Claims (1)
1. a sodium sulfide preparation method, it is characterised in that comprise the following steps: S100: take and produce what barium sulfate produced
Sodium sulfide solution, containing sodium sulfide 40～70g/L in this aqueous solution；S200: add 40～70g/L sulfurations in aqueous
Sodium water solution, more than temperature 70 C, clarifies more than 20 hours, filters clarification；S300: be evaporated to about 250g/L, it is thus achieved that sulfuration
Sodium semi-finished product；S400: beaten to tramp iron separator by sodium sulfide semi-finished product, the many polyiron sulfates adding 0.1-0.3%wt make generation
Various deposits settle, and stir 20 minutes temperature 70～80 DEG C of filtrations；Obtain the iron content sodium sulfide solution at below 1ppm；
S500: the solution evaporation of step S400 is concentrated into 60% content, film-making i.e. obtains iron content and produces at the sodium sulfide of below 10ppm
Product；S600: adding manganese powder and/or manganese-base alloy powder in solution of zinc sulfate, temperature is 50 DEG C and pH ＞ 4.0, and stirring is anti-
Should, after react, filter separate, after through evaporating, concentrating and crystallizing, obtain high-purity sulfuric acid zinc, will prepare high-purity sulfuric acid
Zinc adds zinc sulfate 5-10 kilogram quantities by every cube of filtrate and weighs zinc sulfate, and every cube of filtrate correspondence 1 cube of zinc sulfate of preparation is molten
Liquid；By every cube of water adds barium sulfide 150kg, take clear liquid standby；Solution both the above prepared, is simultaneously introduced sodium sulfide
In filtrate, stirring, reaction temperature controls more than 80 DEG C, precipitation, after remove impurity clarification, send evaporization process, through evaporation and concentration and get final product
To high purity sodium sulfide.
Priority Applications (1)
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| CN201610509025.3A CN106185838A (en) | 2016-07-01 | 2016-07-01 | Sodium sulfide preparation method |
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| CN201610509025.3A CN106185838A (en) | 2016-07-01 | 2016-07-01 | Sodium sulfide preparation method |
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| CN106185838A true CN106185838A (en) | 2016-12-07 |
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| CN201610509025.3A Pending CN106185838A (en) | 2016-07-01 | 2016-07-01 | Sodium sulfide preparation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110155954A (en) * | 2019-04-24 | 2019-08-23 | 贵州红星发展股份有限公司 | A kind of preparation method of high-purity sodium sulfide crystal |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU833565A1 (en) * | 1979-05-31 | 1981-05-30 | Научно-Исследовательский И Проектныйинститут Цветной Металлургии | Method of waste water purification from thiosulfate ion |
| CN1244493A (en) * | 1999-09-13 | 2000-02-16 | 甘肃亚盛盐化工业集团有限责任公司 | Production technology of yellow flaky sodium sulfide with low carbon and iron contents |
| CN101823701A (en) * | 2009-03-04 | 2010-09-08 | 范清玉 | Production technology of sodium sulfide with high purity white crystals |
| CN105714116A (en) * | 2016-03-16 | 2016-06-29 | 中南大学 | Method for removing copper, cadmium, nickel and cobalt out of zinc sulfate solution through one step |
-
2016
- 2016-07-01 CN CN201610509025.3A patent/CN106185838A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU833565A1 (en) * | 1979-05-31 | 1981-05-30 | Научно-Исследовательский И Проектныйинститут Цветной Металлургии | Method of waste water purification from thiosulfate ion |
| CN1244493A (en) * | 1999-09-13 | 2000-02-16 | 甘肃亚盛盐化工业集团有限责任公司 | Production technology of yellow flaky sodium sulfide with low carbon and iron contents |
| CN101823701A (en) * | 2009-03-04 | 2010-09-08 | 范清玉 | Production technology of sodium sulfide with high purity white crystals |
| CN105714116A (en) * | 2016-03-16 | 2016-06-29 | 中南大学 | Method for removing copper, cadmium, nickel and cobalt out of zinc sulfate solution through one step |
Non-Patent Citations (3)
| Title |
|---|
| 刘明华: "《水处理化学品》", 31 January 2010 * |
| 邝生鲁: "《现代精细化工》", 31 December 1997 * |
| 马世昌: "《化学物质辞典》", 30 April 1990 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110155954A (en) * | 2019-04-24 | 2019-08-23 | 贵州红星发展股份有限公司 | A kind of preparation method of high-purity sodium sulfide crystal |
| CN110155954B (en) * | 2019-04-24 | 2021-02-23 | 贵州红星发展股份有限公司 | Preparation method of high-purity sodium sulfide crystal |
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Application publication date: 20161207 |