CN106430113B - A kind of manufacture craft reducing oxidizing sodium sulphide degree - Google Patents
A kind of manufacture craft reducing oxidizing sodium sulphide degree Download PDFInfo
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- CN106430113B CN106430113B CN201610932736.1A CN201610932736A CN106430113B CN 106430113 B CN106430113 B CN 106430113B CN 201610932736 A CN201610932736 A CN 201610932736A CN 106430113 B CN106430113 B CN 106430113B
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- vulcanized sodium
- silica gel
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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
- C01B17/40—Making shaped products, e.g. granules
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- Organic Chemistry (AREA)
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Abstract
This patent discloses a kind of manufacture crafts reducing oxidizing sodium sulphide degree, including material process-calcination process-hot melt, clarify process-press filtration process-evaporation and concentration process, sodium sulfide solution after being concentrated by evaporation process is sent in comminutor, it is 20 30/min to be granulated machine nozzle to spray the speed of vulcanized sodium particle, silica gel balloon is arranged at the nozzle of comminutor, the vulcanized sodium particle sprayed through nozzle, which enters in silica gel balloon, to be removed and closes, then upper new silica gel balloon is covered on nozzle again, after the completion of the cooling of vulcanized sodium particle, packing for vulcanized sodium particle can then be carried out by puncturing silica gel balloon.This programme can effectively reduce vulcanized sodium particle and oxidation occurs when being cooled and shaped and deliquesces phenomenon, greatly improve the quality of production of vulcanized sodium particle.
Description
Technical field
The present invention relates to vulcanized sodium production technical field, specially a kind of manufacture craft of vulcanized sodium.
Background technology
There is strong corrosivity, finished product easily to deliquesce, aoxidize for vulcanized sodium also known as akali sulphide.For the system of vulcanized sodium product
Make：First, using barreled, i.e., the sodium sulfide solution after concentration is directly injected into cooled and solidified in bucket and formed, though this technology of the package
It is so simple, but its shortcoming is extremely inconvenient when using, and after must breaking pail pack, takes out the vulcanized sodium for wherein congealing into monoblock
Solid, also needing to be smashed can use, and labor intensity is big, time-consuming.Second is that by the semi-finished product lye after evaporation and concentration by
Semi-finished product tank is put into pelleter, as the rotation lye of roller is attached to cylinder outer wall, thin layer is formed, because being adopted in pelleter rotary cylinder
It being cooled down with recirculated water, the crystallization and freezing quickly of the vulcanized sodium in lye is detached from by scraper discharging akali sulphide and roller,
Form piece alkali.Both modes when making vulcanized sodium, vulcanized sodium be all easy to the oxygen and reaction of moisture in air, in turn
So that vulcanized sodium is easy to happen deliquescence and the oxidation of product in the production process.
A kind of processing for granular sodium sulfide, including raw material work are disclosed in China Patent No. ZL03152783.3
Bricklayer's's sequence-chemical subtraction process-precipitation process-evaporation and concentration process is washed in sequence-calcination process-heat-welding process-clarification, warp
Sodium sulfide solution after evaporation and concentration, sodium sulfide content >=60% are pumped out by pump, through filter by contaminant filter, into granulation
The sodium sulfide solution temperature of machine head is 130-150 DEG C, 0.3-0.5Mpa of discharge pressure, is sprayed through head nozzle, cold in steel band
But be cooled and shaped on device, the particle discharging after solidification enters in blanking device, vacuum packaging or plastic bag sealing packaging to get at
Product.
Above-mentioned processing for granular sodium sulfide provides prilling item according to the unique physical characteristic of vulcanized sodium concentrate
Part makes vulcanized sodium product realize granulating, and vacuum-packed technique is applied, and effectively reduces the tide of vulcanized sodium product
Solution, oxidation, to extend inventory time, the resting period was up to 2 years or more.But said program still can when producing vulcanized sodium
There is a problem of following：When head nozzle ejection of the sodium sulfide solution through comminutor, when being cooled and shaped in steel belt cooler, at
Vulcanized sodium during type still can in air water and oxygen react so that the vulcanized sodium produced deliquesces and oxygen
Change, this will undoubtedly influence the quality for the vulcanized sodium produced.
Invention content
The invention is intended to provide a kind of making of reduction vulcanized sodium particle generation oxidation and deliquescence degree when being cooled and shaped
Technique.
A kind of manufacture craft of reduction oxidizing sodium sulphide degree in this programme, including material process-calcination process-heat
The concentration of molten, clarification process-press filtration process-evaporation and concentration process, the sodium sulfide solution after evaporation and concentration is more than 65%, will be through
Sodium sulfide solution after pervaporation enrichment process is sent to by the speed of 0.2-0.3L/min in comminutor, reaches comminutor head
The temperature of sodium sulfide solution at nozzle is 100-120 °C, and the speed that nozzle sprays vulcanized sodium particle is 20-30/min,
Silica gel balloon is arranged at the nozzle of comminutor, the vulcanized sodium particle sprayed through nozzle enters directly into silica gel balloon, is equipped with
The silica gel balloon of vulcanized sodium particle is removed and is closed from nozzle, then covers upper new silica gel balloon on nozzle again, so past
Multiple, each vulcanized sodium particle sprayed from nozzle is encased in a silica gel balloon, after the completion of the cooling of vulcanized sodium particle, thorn
Broken silica gel balloon can then carry out packing for vulcanized sodium particle.
When making granular vulcanized sodium using this programme, the sodium sulfide solution after evaporation and concentration is sent in comminutor
It is granulated, silica gel balloon is arranged on the nozzle of comminutor, silica gel balloon has higher heat resistance, sprayed through comminutor
The vulcanized sodium particle that mouth sprays enters directly into silica gel balloon, and at this time under the action of vulcanized sodium particle, silica gel balloon will be sent out
The variation of raw body product, which will be the volume of silica gel balloon, to become larger, and vulcanized sodium particle will fit closely between silica gel balloon and will discharge
Air in silica gel balloon is removed silica gel balloon and is sealed at this time, then upper new silica gel balloon is covered on nozzle, so
Back and forth, each vulcanized sodium particle is placed in a silica gel balloon and is cooled down, when needing to pack to vulcanized sodium particle
When, it punctures silica gel balloon and takes out vulcanized sodium particle, then the vulcanized sodium particle is sealed guarantee.
The effect of this programme is：This programme utilizes the heat resistance and elastic property of silica gel balloon, the sulphur that will be produced
Change sodium particle to be directly introduced in silica gel balloon, sky while vulcanized sodium particle struts silica gel balloon in discharge silica gel balloon
Gas, such vulcanized sodium particle will not be contacted when being cooled and shaped in silica gel balloon with air, also would not in air
Moisture and oxygen reaction and generate deliquesce and oxidation the phenomenon that.Therefore this programme can effectively reduce vulcanized sodium particle and be cooled to
Oxidation occurs when type and deliquesces phenomenon, greatly improves the quality of production of vulcanized sodium particle.
Further, the steel band of movement is equipped in the lower section for being granulated machine nozzle, the steel band back side is connected with cooling water, the stream of cooling water
Amount is 1-1.5L/min, is placed on steel band after removing the silica gel balloon that vulcanized sodium particle is housed from nozzle, the steel band back side
Cooling water cooling effect is played to the vulcanized sodium particle in silica gel balloon, the silica gel balloon equipped with vulcanized sodium particle cooled down
Steel band through movement is transported at product packaging and is packed.It is cold in the vulcanized sodium particle progress to being fitted into silica gel balloon
When but, the cooling water that the steel band back side is passed through can accelerate the cooling of vulcanized sodium particle, meanwhile, the steel band of movement can be by vulcanized sodium particle
It is automatically sent at packaging, improves the degree of automation of whole process.
Further, in being concentrated by evaporation process, the temperature of evaporation and concentration is 130-150 °C.The temperature so that vulcanized sodium is molten
Liquid energy is evaporated faster, improves the entire efficiency for being concentrated by evaporation process.
Further, the sodium sulfide solution after being concentrated by evaporation process is sent to comminutor by the speed of 0.2L/min
In, the speed for being granulated the vulcanized sodium particle that machine nozzle sprays is 20/min.Vulcanized sodium is sprayed with the speed of 20/min to be made
There is time enough to take out the silica gel balloon for being packed into vulcanized sodium particle from nozzle and cover upper new silica gel balloon, while again will not
Since speed influences the granulation speed of vulcanized sodium particle slowly excessively.
Further, the flow of cooling water is 1.5L/min.The cooling water of the flow can preferably meet vulcanized sodium on steel band
Cooling requirement so that can just cool down and be packed when vulcanized sodium particle is transported to from steel band from packaging.
Specific implementation mode
Below by specific implementation mode, the present invention is described in further detail：
Embodiment 1：
A kind of manufacture craft reducing oxidizing sodium sulphide degree, includes the following steps：
（1）, material process：Feed coal and saltcake are crushed, broken grain size is less than 5mm, and presses 1:2 ratio
Broken feed coal and saltcake are mixed；
（2）, calcination process：By step（1）In raw material by feeding device from the tail portion of kiln be added kiln in, kiln hood
Place is added in kiln using coal dust adverse current and is heated to kiln, and the temperature in kiln is 1100 °C, and raw material is burnt into kiln
Clinker；
（3）, hot melt, clarification process：By step（2）The clinker of middle firing is added to by kiln hood in hot melt jar, be used in combination containing
The thermokalite water of a small amount of vulcanized sodium is leached, and the vulcanized sodium in clinker, which enters in thermokalite water, forms turbid lye, insoluble particle by
Hot melt jar lower part is drained into washery slag tank and is washed；
（4）, press filtration process：By step（4）In turbid lye be put into filter press the liquid for being separated by solid-liquid separation, being isolated
Body is the higher high alkali liquid of sodium sulfide content, the further press filtration recycling vulcanized sodium of the solid isolated；
（5）, be concentrated by evaporation process：By step（4）In obtained high alkali liquid be put into evaporator and be evaporated concentration, steam
The temperature of hair concentration is 130 °C, and the concentration of the sodium sulfide solution after evaporation and concentration is more than 65%；
（6）Granulating working procedure：Sodium sulfide solution after being concentrated by evaporation process is sent to by the speed of 0.2L/min and is made
In grain machine, the temperature for reaching the sodium sulfide solution at comminutor head nozzle is 100 °C, and nozzle sprays the speed of vulcanized sodium particle
For 20/min, silica gel balloon is arranged at the nozzle of comminutor, the vulcanized sodium particle sprayed through nozzle enters directly into silicon
In glue balloon, the silica gel balloon equipped with vulcanized sodium particle is removed and is closed from nozzle, then covers upper new silicon on nozzle again
Glue balloon is equipped with the steel band of movement in the lower section for being granulated machine nozzle, and the steel band back side is connected with cooling water, and the flow of cooling water is 1L/
Min is placed on after removing the silica gel balloon that vulcanized sodium particle is housed from nozzle on steel band, and the cooling water at the steel band back side is to silicon
Vulcanized sodium particle in glue balloon plays cooling effect, and and so on, each vulcanized sodium particle sprayed from nozzle is encased in
In one silica gel balloon, steel band of the silica gel balloon through movement equipped with vulcanized sodium particle cooled down is transported at product packaging,
Packing for vulcanized sodium particle can then be carried out by puncturing silica gel balloon.
Embodiment 2：
A kind of manufacture craft reducing oxidizing sodium sulphide degree, includes the following steps：
（1）, material process：Feed coal and saltcake are crushed, broken grain size is less than 3mm, and presses 1:2 ratio
Broken feed coal and saltcake are mixed；
（2）, calcination process：By step（1）In raw material by feeding device from the tail portion of kiln be added kiln in, kiln hood
Place is added in kiln using coal dust adverse current and is heated to kiln, and the temperature in kiln is 1050 °C, and raw material is burnt into kiln
Clinker；
（3）, hot melt, clarification process：By step（2）The clinker of middle firing is added to by kiln hood in hot melt jar, be used in combination containing
The thermokalite water of a small amount of vulcanized sodium is leached, and the vulcanized sodium in clinker, which enters in thermokalite water, forms turbid lye, insoluble particle by
Hot melt jar lower part is drained into washery slag tank and is washed；
（4）, press filtration process：By step（4）In turbid lye be put into filter press the liquid for being separated by solid-liquid separation, being isolated
Body is the higher high alkali liquid of sodium sulfide content, the further press filtration recycling vulcanized sodium of the solid isolated；
（5）, be concentrated by evaporation process：By step（4）In obtained high alkali liquid be put into evaporator and be evaporated concentration, steam
The temperature of hair concentration is 150 °C, and the concentration of the sodium sulfide solution after evaporation and concentration is more than 65%；
（6）Granulating working procedure：Sodium sulfide solution after being concentrated by evaporation process is sent to by the speed of 0.25L/min and is made
In grain machine, the temperature for reaching the sodium sulfide solution at comminutor head nozzle is 110 °C, and nozzle sprays the speed of vulcanized sodium particle
For 25/min, silica gel balloon is arranged at the nozzle of comminutor, the vulcanized sodium particle sprayed through nozzle enters directly into silicon
In glue balloon, the silica gel balloon equipped with vulcanized sodium particle is removed and is closed from nozzle, then covers upper new silicon on nozzle again
Glue balloon is equipped with the steel band of movement in the lower section for being granulated machine nozzle, and the steel band back side is connected with cooling water, and the flow of cooling water is
1.5L/min is placed on after removing the silica gel balloon that vulcanized sodium particle is housed from nozzle on steel band, the cooling at the steel band back side
Water plays cooling effect to the vulcanized sodium particle in silica gel balloon, and and so on, each vulcanized sodium particle sprayed from nozzle is equal
It is encased in a silica gel balloon, steel band of the silica gel balloon through movement equipped with vulcanized sodium particle cooled down is transported to product packet
At dress, packing for vulcanized sodium particle can then be carried out by puncturing silica gel balloon.
Comparative example:
Bricklayer's is washed in a kind of processing for granular sodium sulfide, including material process-calcination process-heat-welding process-clarification
Sequence-chemical subtraction process-precipitation process-evaporation and concentration process, the sodium sulfide solution after evaporation and concentration, sodium sulfide content
>=60%, it is pumped out by pump, through filter by contaminant filter, the sodium sulfide solution temperature into comminutor head is 130-150 DEG C,
0.3-0.5Mpa of discharge pressure, through head nozzle spray, be cooled and shaped in steel belt cooler, the particle discharging after solidification into
Enter in blanking device, vacuum packaging or plastic bag sealing packaging are to get finished product.
The graininess vulcanized sodium that embodiment 1, embodiment 2 and comparative example produce 100, and to producing is respectively adopted
Granular vulcanized sodium carries out the detection of oxidizability and deliquescence degree, obtains that the results are shown in table below：
| Embodiment 1 | Embodiment 2 | Comparative example | |
| Occur oxidation or（With）The quantity of the vulcanized sodium of deliquescence | 5 | 3 | 30 |
| The maximum oxidation area occupation ratio of single vulcanized sodium | 10% | 8% | 45% |
| The most great talent of single vulcanized sodium deliquesces area occupation ratio | 7% | 5% | 38% |
The graininess vulcanized sodium produced using this programme embodiment 1 and embodiment 2 it can be seen from the data in upper table
The reduction for the high number for deliquescing and aoxidizing occurs, slip reaches 83% or more, while single vulcanized sodium occurs oxidation or deliquesces
Maximum area rate also decline to a great extent, therefore this programme can effectively reduce vulcanized sodium particle oxidation and deliquesce phenomenon, greatly
Improve the vulcanized sodium quality produced, improve product competitiveness in the market.
Above-described is only the embodiment of the present invention, and the common sense such as well known concrete structure and characteristic are not made herein in scheme
Excessive description.It, without departing from the structure of the invention, can be with it should be pointed out that for those skilled in the art
Several modifications and improvements are made, these should also be considered as protection scope of the present invention, these all do not interfere with what the present invention was implemented
Effect and patent practicability.The scope of protection required by this application should be based on the content of the claims, in specification
The records such as specific implementation mode can be used for explaining the content of claim.
Claims (4)
1. a kind of manufacture craft reducing oxidizing sodium sulphide degree, including material process-calcination process-hot melt, clarification work
Sequence-press filtration process-evaporation and concentration process, which is characterized in that the concentration of the sodium sulfide solution after evaporation and concentration is more than 65%, will
Sodium sulfide solution after being concentrated by evaporation process is sent to by the speed of 0.2-0.3L/min in comminutor, reaches comminutor machine
The temperature of sodium sulfide solution at head nozzle is 100-120 DEG C, and the speed that nozzle sprays vulcanized sodium particle is 20-30/min,
It is arranged with silica gel balloon at the nozzle of comminutor, is equipped with the steel band of movement in the lower section for being granulated machine nozzle, the steel band back side is connected with
The flow of cooling water, cooling water is 1-1.5L/min；The vulcanized sodium particle sprayed through nozzle enters directly into silica gel balloon, fills
There is the silica gel balloon of vulcanized sodium particle to remove and close from nozzle, then covers upper new silica gel balloon on nozzle again, so
Back and forth, each vulcanized sodium particle sprayed from nozzle is encased in a silica gel balloon, after the completion of the cooling of vulcanized sodium particle,
It is placed on steel band after silica gel balloon equipped with vulcanized sodium particle is removed from nozzle, the cooling water at the steel band back side is to silica gel balloon
Interior vulcanized sodium particle plays cooling effect, and steel band of the silica gel balloon through movement equipped with vulcanized sodium particle cooled down is transported to
At product packaging, packing for vulcanized sodium particle can then be carried out by puncturing silica gel balloon.
2. the manufacture craft according to claim 1 for reducing oxidizing sodium sulphide degree, it is characterised in that：It is being concentrated by evaporation work
In sequence, the temperature of evaporation and concentration is 130-150 DEG C.
3. the manufacture craft according to claim 1 for reducing oxidizing sodium sulphide degree, it is characterised in that：It will be dense through pervaporation
Sodium sulfide solution after contracting process is sent to by the speed of 0.2L/min in comminutor, is granulated the vulcanized sodium particle that machine nozzle sprays
Speed be 20/min.
4. the manufacture craft according to claim 2 for reducing oxidizing sodium sulphide degree, it is characterised in that：The flow of cooling water
For 1.5L/min.
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| CN201610932736.1A CN106430113B (en) | 2016-10-31 | 2016-10-31 | A kind of manufacture craft reducing oxidizing sodium sulphide degree |
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| CN109455676B (en) * | 2019-01-21 | 2022-05-27 | 范冲天 | Environment-friendly refining method of sodium sulfide |
| CN110240181A (en) * | 2019-06-06 | 2019-09-17 | 浙江天地环保科技有限公司 | A kind of dehydration and drying system and method freezing saltcake |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN1257829A (en) * | 1998-12-20 | 2000-06-28 | 内蒙古伊克昭化工研究设计院 | Process for granulating sodium sulfide |
| CN1485268A (en) * | 2003-08-18 | 2004-03-31 | 甘肃亚盛盐化工业集团有限责任公司 | Processing for granular sodium sulfide |
| CN103418159A (en) * | 2013-05-09 | 2013-12-04 | 青岛科技大学 | New method for preventing nano particles from re-agglomerating during rapid expansion of supercritical fluid |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6582675B2 (en) * | 2000-03-28 | 2003-06-24 | Degussa Ag | Method for the preparation of anhydrous sodium sulfide |
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- 2016-10-31 CN CN201610932736.1A patent/CN106430113B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1257829A (en) * | 1998-12-20 | 2000-06-28 | 内蒙古伊克昭化工研究设计院 | Process for granulating sodium sulfide |
| 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 |
| CN1485268A (en) * | 2003-08-18 | 2004-03-31 | 甘肃亚盛盐化工业集团有限责任公司 | Processing for granular sodium sulfide |
| CN103418159A (en) * | 2013-05-09 | 2013-12-04 | 青岛科技大学 | New method for preventing nano particles from re-agglomerating during rapid expansion of supercritical fluid |
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Effective date of registration: 20201202 Address after: No. 1415 Shouxiang Avenue, Bama Town, Bama Yao Autonomous County, Hechi City, Guangxi Zhuang Autonomous Region Patentee after: Zhu Rong Address before: 408422 Chongqing city Nanping Town, Nanchuan District Village Flower agency Patentee before: CHONGQING CITY NANCHUAN DISTRICT QINGYAN WELFARE ALKALI FACTORY |
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Effective date of registration: 20211228 Address after: 402660 plot d19-5 / 02, North District, industrial park, Tongnan District, Chongqing Patentee after: Chongqing Liyuan Chemical Co.,Ltd. Address before: 1415 Shouxiang Avenue, Bama Town, Bama Yao Autonomous County, Hechi City, Guangxi Zhuang Autonomous Region 547599 Patentee before: Zhu Rong |