CN1308013A - Preparation process of anhydrous sodium sulfide crystal - Google Patents
Preparation process of anhydrous sodium sulfide crystal Download PDFInfo
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- CN1308013A CN1308013A CN 00137133 CN00137133A CN1308013A CN 1308013 A CN1308013 A CN 1308013A CN 00137133 CN00137133 CN 00137133 CN 00137133 A CN00137133 A CN 00137133A CN 1308013 A CN1308013 A CN 1308013A
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- sodium sulfide
- crystal
- drying
- sulfide crystal
- moisture
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The preparation method of anhydrous sodium sulfide crystal includes the following steps: adding adjuvant into coal powder and adopting sodium sulfate reduction process to prepare sodium sulfide solution, removing impurity and crystallizing to obtain sodium sulfide crystal containing 9 crystal waters or 5.5 crystal waters, then under the condition of reduced pressure heating and drying. It is characterized by that the drying temp. of close related to pressure, so that it can prevent aqua compound from producing condensation or adhering to the drier. The anhydrous sodium sulfide crystal obtained by using said invented method features high purity, large specific surface area and uniform granules, and can completely meet the requirements for quality of anhydrous sodium sulfide when the polyphenylene thioether is synthesized.
Description
The present invention relates to a kind of production technique of sodium sulphite, especially a kind of preparation method of Sodium sulphate anhydrous, 99min.
Producing Sodium sulphate anhydrous, 99min generally has two kinds of approach, and the one, use H
2, CO, CH
4Reduce anhydrous sodium sulphate directly obtain under certain temperature and pressure Deng gas, this method is because the bad grasp of reaction conditions, poor stability, and quality product is also unstable, is difficult to enter suitability for industrialized production.Another kind of approach is to adopt coal dust reduction sodium sulfate (saltcake), makes sodium sulfide solution after the leaching, and evaporation or crystallization after drying obtain Sodium sulphate anhydrous, 99min.Sodium sulfide solution evaporate to dryness gained Sodium sulphate anhydrous, 99min is generally powdery or bulk, and it is bad to be used for the polyphenylene sulfide synthetic effect.Sodium sulphite crystallizing and drying system Sodium sulphate anhydrous, 99min has two kinds of methods, and a kind of is to be thermal source with rare gas element (as nitrogen), under reduced state, with sulfuration bed fluidized drying, though this method thermo-efficiency height, rate of drying is fast, but because that sodium sulfide crystal dissolves is a little low, the bad control of temperature is easily lumpd.Another kind of drying means is vacuum-drying, sodium sulfide crystal is placed in the Vacuumdrier, adopt heat-conducting oil heating, under extremely low vacuum condition, boiling point descends, at low temperatures, crystal water can break away from crystal and become water vapour and be drawn out of, thereby has avoided hydrate to take place coalescent or be bonded on the moisture eliminator gained anhydrous sodium sulfide crystal, have characteristics such as uniform particles, specific surface area be big, can satisfy the requirement of polyphenylene sulfide synthetic fully.
The present invention promptly adopts moisture sodium sulfide crystal vacuum-drying to prepare anhydrous sodium sulfide crystal.Concrete processing step is as follows:
Auxiliary agent is added in the sodium sulfide solution that coal dust reduction sodium sulfate makes, remove partial impurities after filtration, the sodium sulfide solution concentration after the removal of impurities should be controlled at 24wt.%-35wt.%, is stirring crystallisation by cooling under the companion then, make in the sodium sulfide crystal that contains 5.5-9 crystal water any, preferred Na
2S
5.5H
2O.
Moisture sodium sulfide crystal is placed in rake formula or the rotary-drum vacuum drying machine, control pressure＜15 holder, temperature continues by 20-30 ℃ or intermittent warming treatment to 97 ℃ or low slightly, 2 hours time of drying or longer.Rising pressure continues to be warming up to 200 ℃ or higher.Treat in the sodium sulphite that moisture content is less than being cooled to 40 ℃ or lower packing at 0.5% o'clock.
Advantage of the present invention is: the anhydrous sodium sulfide crystal that makes has purity height, big, the uniform particles of specific surface area, can satisfy the requirement of polyphenylene sulfide (PPS) synthetic fully.
Further specify content of the present invention below by embodiment:
With the sodium sulfide solution of concentration 33wt.% crystallisation by cooling under agitation, make the moisture sodium sulfide crystal that contains 5.5-6 crystal water, place rake formula Vacuumdrier inner control pressure＜15 holders, continue or intermittent warming treatment to 97 ℃ 2 hours time of drying or longer, 15 holders or higher of rising pressure by initial 20-30 ℃, continue to be warming up to 210 ℃, stop heating, be cooled to 30 ℃, normal pressure is packing down.
Anhydrous sodium sulfide crystal quality index by method for preparing is as follows:
Sodium sulphite (Na
2S) content 〉=94wt.%
Moisture content≤0.5wt.%
Sulfothiorine (Na
2S
2O
3) and
S-WAT (Na
2SO
3)≤2.5wt.%
Iron (Fe) content≤0.002wt.%
Density≤0.5g/cm
3
Outward appearance: light yellow solid particle.
Claims (7)
1, utilize moisture sodium sulfide crystal to prepare the method for anhydrous sodium sulfide crystal, auxiliary agent added in the sodium sulfide solution that coal dust reduction sodium sulfate produces remove impurity such as yellow soda ash, sodium sulfate, iron, it is characterized in that the sodium sulfide solution after the removal of impurities needs crystallisation by cooling to make moisture sodium sulfide crystal, moisture sodium sulfide crystal is placed Vacuumdrier internal heating drying, slough moisture content, gained anhydrous crystalline cooling back packing.
2, method according to claim 1 is characterized in that described moisture sodium sulfide crystal can be to contain in the moisture sodium sulfide crystal of 5.5-9 crystal water any, preferred Na
2S5.5H
2O.
3, method according to claim 1 is characterized in that drying machine can be rake formula Vacuumdrier and rotary-drum vacuum drying machine.
4, according to the method for claim 1 or 3, it is characterized in that the pressure in the Vacuumdrier begins time＜15 holder, when drying is finished discharging normal pressure.
5, according to the method for claim 1 or 3,20-30 ℃ when it is characterized in that the interior temperature of Vacuumdrier from charging is persistently overheating to 200 ℃ or higher.
6, according to the method for claim 1-5, it is characterized in that drying finish after temperature of charge need be cooled to 40 ℃ or can discharging when lower.
7, according to the method for claim 1-6, it is characterized in that the sodium sulphite that produces be powdery and granular in any, it is light yellow that outward appearance is, sodium sulfide content is 94wt.% at least, density＜0.6g/cm
3
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00137133 CN1308013A (en) | 2000-12-30 | 2000-12-30 | Preparation process of anhydrous sodium sulfide crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00137133 CN1308013A (en) | 2000-12-30 | 2000-12-30 | Preparation process of anhydrous sodium sulfide crystal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1308013A true CN1308013A (en) | 2001-08-15 |
Family
ID=4597683
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 00137133 Pending CN1308013A (en) | 2000-12-30 | 2000-12-30 | Preparation process of anhydrous sodium sulfide crystal |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1308013A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104163402A (en) * | 2014-07-18 | 2014-11-26 | 中国石油化工股份有限公司 | Preparation method of anhydrous sodium sulfide |
| 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 |
| CN106517100A (en) * | 2016-11-28 | 2017-03-22 | 吴迎喜 | Preparation method of anhydrous sodium sulfide |
-
2000
- 2000-12-30 CN CN 00137133 patent/CN1308013A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104163402A (en) * | 2014-07-18 | 2014-11-26 | 中国石油化工股份有限公司 | Preparation method of anhydrous sodium sulfide |
| 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 |
| CN106517100A (en) * | 2016-11-28 | 2017-03-22 | 吴迎喜 | Preparation method of anhydrous sodium sulfide |
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |