CN116924344B - Granulating method of sodium hydrosulfide - Google Patents
Granulating method of sodium hydrosulfide Download PDFInfo
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- CN116924344B CN116924344B CN202311194015.1A CN202311194015A CN116924344B CN 116924344 B CN116924344 B CN 116924344B CN 202311194015 A CN202311194015 A CN 202311194015A CN 116924344 B CN116924344 B CN 116924344B
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- HYHCSLBZRBJJCH-UHFFFAOYSA-M sodium hydrosulfide Chemical compound [Na+].[SH-] HYHCSLBZRBJJCH-UHFFFAOYSA-M 0.000 title claims abstract description 157
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000002245 particle Substances 0.000 claims abstract description 74
- 238000005469 granulation Methods 0.000 claims abstract description 17
- 230000003179 granulation Effects 0.000 claims abstract description 17
- 239000007921 spray Substances 0.000 claims abstract description 10
- 238000005507 spraying Methods 0.000 claims description 47
- 239000007787 solid Substances 0.000 claims description 43
- IHYNKGRWCDKNEG-UHFFFAOYSA-N n-(4-bromophenyl)-2,6-dihydroxybenzamide Chemical compound OC1=CC=CC(O)=C1C(=O)NC1=CC=C(Br)C=C1 IHYNKGRWCDKNEG-UHFFFAOYSA-N 0.000 claims description 42
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 35
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 35
- 230000006911 nucleation Effects 0.000 claims description 33
- 238000010899 nucleation Methods 0.000 claims description 33
- 239000007864 aqueous solution Substances 0.000 claims description 25
- 238000001914 filtration Methods 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 20
- 239000000155 melt Substances 0.000 claims description 18
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 10
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 9
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 7
- 229910052742 iron Inorganic materials 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 238000002203 pretreatment Methods 0.000 claims description 2
- 150000001339 alkali metal compounds Chemical class 0.000 abstract description 2
- 238000010521 absorption reaction Methods 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 17
- 238000005303 weighing Methods 0.000 description 13
- 239000002667 nucleating agent Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 4
- 238000009826 distribution Methods 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000012824 chemical production Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethanethiol Chemical compound CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000000543 intermediate Substances 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 239000010985 leather Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000000988 sulfur dye Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- UYJXRRSPUVSSMN-UHFFFAOYSA-P ammonium sulfide Chemical compound [NH4+].[NH4+].[S-2] UYJXRRSPUVSSMN-UHFFFAOYSA-P 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007380 fibre production Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 238000005453 pelletization Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000011265 semifinished product Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Glanulating (AREA)
Abstract
The invention discloses a granulating method of sodium hydrosulfide, belonging to the field of alkali metal compounds. The method comprises the steps of melt pretreatment and spray thermal bonding granulation, and the granulation method of the invention ensures that the particle size of the prepared sodium hydrosulfide particles is more concentrated, the proportion of particles below 0.2mm is 3.38-3.57%, the proportion of particles below 0.2-0.5mm is 10.96-12.07%, the proportion of particles below 0.5-1.0mm is 78.25-79.03%, the proportion of particles above 1.0-1.5mm is 4.73-5.34%, and the proportion of particles above 1.5mm is 1.09-1.78%.
Description
Technical Field
The invention relates to a granulating method of sodium hydrosulfide, belonging to the field of alkali metal compounds.
Background
Sodium hydrosulfide is a new chemical raw material after sodium sulfide, and has the basic characteristics and functions of sodium sulfide, and almost all sodium hydrosulfide exists in the form of sulfhydryl in water, so that the ion concentration is correspondingly higher than that of sodium sulfide, and therefore, the sodium hydrosulfide has more excellent performance in the chemical field.
Sodium hydrosulfide is a raw material for preparing ammonium sulfide and pesticide ethanethiol semi-finished products, is also an auxiliary agent for synthesizing organic intermediates and preparing sulfur dyes in the fuel industry, can be used for synthesizing organic intermediates and preparing sulfur dyes, can be used for tanning leather of leather industry peltry, can be used for water treatment, is largely used for copper ore dressing in mining industry, and is used for sulfurous acid dyeing in artificial fiber production, and the like.
The present solid sodium bisulfide product mainly takes flaky solid as main material, the principle is that dehydrated sodium bisulfide solution is cooled to a certain extent and cooled and solidified to form solid sodium bisulfide, CN1207182A discloses a production method of flaky sodium bisulfide, the obtained sodium bisulfide solution is concentrated and insulated, the concentrated sodium bisulfide solution is sent to the surface of a roller medium-cooling type pelleter, cooling water is introduced into medium-cooling holes of the rotary roller, sodium bisulfide on the surface of the roller is solidified, and finally irregular flaky sodium bisulfide is scraped by a scraper. CN109956456a discloses a method for purifying sodium bisulfide, which comprises the steps of delivering molten sodium bisulfide separated from crystal salt into a vacuum heat preservation tank for heat preservation, delivering the molten sodium bisulfide into a vacuum rake cooler through a pump for cooling and solidifying into a flake shape, and finally obtaining the flake sodium bisulfide.
In any method for preparing the flaky sodium hydrosulfide, the finally obtained flaky solid is irregular, and has great difference in thickness and area of the sodium hydrosulfide, and although the national standard does not limit the shape specification of the flaky sodium hydrosulfide, in practical application, the flaky sodium hydrosulfide still has a certain influence on the chemical production using the sodium hydrosulfide, in addition, the flaky sodium hydrosulfide is easy to absorb moisture, and the content of the flaky sodium hydrosulfide is extremely easy to be reduced due to intolerance to storage, so that the flaky sodium hydrosulfide cannot be used finally.
At present, no mature technology for producing sodium hydrosulfide particles by a granulating method exists in the market, the applicant tries to granulate sodium hydrosulfide solution so as to improve the moisture absorption resistance of sodium hydrosulfide solids and reduce the inconvenience brought by flaky sodium hydrosulfide to production, and in the process of trying to produce sodium hydrosulfide particles, the moisture absorption resistance is found to be improved greatly compared with flaky sodium hydrosulfide, but the particle size interval of the particles is larger, the particle size of the particles is uneven, bubbles are generated in the particles, and the chemical production using sodium hydrosulfide is still influenced to a certain extent.
In summary, in the prior art, the flaky sodium hydrosulfide is easy to absorb moisture, and the flaky sodium hydrosulfide can bring a certain degree of inconvenience to production, and the sodium hydrosulfide particles are produced by a granulating method, so that the moisture absorption resistance of sodium hydrosulfide solids can be improved, but the produced sodium hydrosulfide particles have uneven particle size, and bubbles can be generated in the particles.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, and prepares sodium hydrosulfide for nucleation by pretreating a melt, and then uses the sodium hydrosulfide as a nucleating agent to granulate with the melt sodium hydrosulfide, so that the particle size of the sodium hydrosulfide particles is more concentrated and the generation of bubbles in the particles is reduced while the moisture absorption resistance of the sodium hydrosulfide particles is improved.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for granulating sodium hydrosulfide, which comprises the steps of melt pretreatment and spray thermal bonding granulation.
The following is a further improvement of the above technical scheme:
the melt pretreatment method comprises the steps of filtering melt sodium hydrosulfide through alumina ceramic, wherein the filtering pressure is 1.60-1.70MPa, the filtering temperature is 131-142 ℃, and the pretreated melt sodium hydrosulfide is obtained after filtering;
the concentration of the melt sodium hydrosulfide is 69-71wt%;
the alumina content of the alumina ceramic was 91.4wt% and the porosity was 83.6%.
The step of spray thermal bonding granulation comprises the steps of preparing sodium hydrosulfide for nucleation and granulating;
spraying a polyvinyl alcohol aqueous solution on solid sodium hydrosulfide, controlling the spraying temperature of the polyvinyl alcohol aqueous solution to be 63-67 ℃, controlling the spraying amount of the polyvinyl alcohol aqueous solution to be 1.8-2.1wt% of the solid sodium hydrosulfide per minute, controlling the temperature of the solid sodium hydrosulfide to be 84-91 ℃ during spraying, continuously stirring while spraying, ending stirring after spraying, heating the sprayed solid sodium hydrosulfide in a nitrogen atmosphere, controlling the heating temperature to be 92-103 ℃, controlling the heating time to be 175-210min, and crushing the solid sodium hydrosulfide to 20-30 mu m after heating to obtain the sodium hydrosulfide for nucleation;
the mass ratio of the solid sodium hydrosulfide to the polyvinyl alcohol aqueous solution is 5:11-13;
the concentration of the polyvinyl alcohol in the polyvinyl alcohol aqueous solution is 0.4-0.6wt% and the molecular weight of the polyvinyl alcohol is 53000-65000;
in the solid sodium hydrosulfide, the content of sodium hydrosulfide is 72.5%, the content of crystal water is 24.4%, the content of iron is 0.00011%, and the content of sodium sulfide is 2.1%;
spraying pretreated melt sodium bisulfide and sodium bisulfide for nucleation into a granulating tower together, fully mixing the pretreated melt sodium bisulfide and the sodium bisulfide for nucleation, controlling the granulating temperature to be 102-107 ℃, controlling the granulating pressure to be 1.32-1.41MPa, cooling after granulating, and cooling to be 9-11 ℃ to obtain sodium bisulfide particles;
the spraying speed of the sodium hydrosulfide in the pretreated melt is 450-550mL/min, the spraying temperature of the sodium hydrosulfide in the pretreated melt is 131-142 ℃, and the diameter of a sodium hydrosulfide nozzle in the pretreated melt is 0.25-0.35mm;
the spraying speed of the sodium hydrosulfide for nucleation is 60-70g/min.
Compared with the prior art, the invention has the following beneficial effects:
according to the granulating method, the particle sizes of the prepared sodium hydrosulfide particles are more concentrated, the proportion of particles below 0.2mm is 3.38-3.57%, the proportion of particles below 0.2-0.5mm is 10.96-12.07%, the proportion of particles below 0.5-1.0mm is 78.25-79.03%, the proportion of particles above 1.0-1.5mm is 4.73-5.34%, and the proportion of particles above 1.5mm is 1.09-1.78%;
the granulating method can improve the moisture absorption resistance of sodium hydrosulfide particles, and the moisture absorption test is carried out in a constant temperature and humidity box for 3 hours, wherein the moisture absorption percentage is 0.64-0.71%, and no caking or aggregation is generated among the particles;
the granulation method can reduce the generation of bubbles in the sodium hydrosulfide particles, and the proportion of the sodium hydrosulfide particles containing the bubbles is 2.31-2.58 percent.
Detailed Description
Example 1
(1) Melt pretreatment
Filtering the melt sodium hydrosulfide by alumina ceramic, wherein the filtering pressure is 1.65MPa, the filtering temperature is 135 ℃, and the pretreated melt sodium hydrosulfide is obtained after the filtering;
the concentration of the melt sodium hydrosulfide is 70wt%;
the alumina content of the alumina ceramic was 91.4wt% and the porosity was 83.6%.
(2) Spray thermal bonding granulation
a. Preparation of sodium hydrosulfide for nucleation
Spraying a polyvinyl alcohol aqueous solution on solid sodium hydrosulfide, controlling the spraying temperature of the polyvinyl alcohol aqueous solution to be 65 ℃, controlling the spraying amount of the polyvinyl alcohol aqueous solution to be 2.0wt% of the solid sodium hydrosulfide per minute, controlling the temperature of the solid sodium hydrosulfide to be 87 ℃ during spraying, continuously stirring while spraying, ending stirring after spraying, heating the sprayed solid sodium hydrosulfide in a nitrogen atmosphere, controlling the heating temperature to be 95 ℃, controlling the heating time to be 180min, and crushing the solid sodium hydrosulfide to 25 mu m after heating to obtain sodium hydrosulfide for nucleation;
the mass ratio of the solid sodium hydrosulfide to the polyvinyl alcohol aqueous solution is 5:12;
the concentration of the polyvinyl alcohol in the polyvinyl alcohol aqueous solution is 0.5 weight percent, and the molecular weight of the polyvinyl alcohol is 58000;
in the solid sodium hydrosulfide, the content of sodium hydrosulfide is 72.5%, the content of crystal water is 24.4%, the content of iron is 0.00011%, and the content of sodium sulfide is 2.1%;
b. granulating
Spraying the pretreated melt sodium bisulfide and sodium bisulfide for nucleation into a granulating tower together, fully mixing the pretreated melt sodium bisulfide and the sodium bisulfide for nucleation, controlling the granulating temperature to be 104 ℃, controlling the granulating pressure to be 1.35MPa, cooling after granulating, and cooling to be 10 ℃ to obtain sodium bisulfide particles;
the spraying speed of the sodium hydrosulfide in the pretreated melt is 500mL/min, the spraying temperature of the sodium hydrosulfide in the pretreated melt is 135 ℃, and the diameter of a sodium hydrosulfide nozzle of the pretreated melt is 0.30mm;
the injection rate of the sodium hydrosulfide for nucleation is 65g/min.
Example 2
(1) Melt pretreatment
Filtering the melt sodium hydrosulfide by alumina ceramic, wherein the filtering pressure is 1.60MPa, the filtering temperature is 142 ℃, and the pretreated melt sodium hydrosulfide is obtained after filtering;
the concentration of the melt sodium hydrosulfide is 71wt%;
the alumina content of the alumina ceramic was 91.4wt% and the porosity was 83.6%.
(2) Spray thermal bonding granulation
a. Preparation of sodium hydrosulfide for nucleation
Spraying a polyvinyl alcohol aqueous solution on solid sodium hydrosulfide, controlling the spraying temperature of the polyvinyl alcohol aqueous solution to be 63 ℃, controlling the spraying amount of the polyvinyl alcohol aqueous solution to be 2.1 weight percent of the solid sodium hydrosulfide per minute, controlling the temperature of the solid sodium hydrosulfide to be 84 ℃ during spraying, continuously stirring while spraying, ending stirring after spraying, heating the sprayed solid sodium hydrosulfide in a nitrogen atmosphere, controlling the heating temperature to be 92 ℃, controlling the heating time to be 210min, and crushing the solid sodium hydrosulfide to 20 mu m after heating to obtain sodium hydrosulfide for nucleation;
the mass ratio of the solid sodium hydrosulfide to the polyvinyl alcohol aqueous solution is 5:11;
the concentration of the polyvinyl alcohol in the polyvinyl alcohol aqueous solution is 0.6wt% and the molecular weight of the polyvinyl alcohol is 53000;
in the solid sodium hydrosulfide, the content of sodium hydrosulfide is 72.5%, the content of crystal water is 24.4%, the content of iron is 0.00011%, and the content of sodium sulfide is 2.1%;
b. granulating
Spraying the pretreated melt sodium bisulfide and sodium bisulfide for nucleation into a granulating tower together, fully mixing the pretreated melt sodium bisulfide and the sodium bisulfide for nucleation, controlling the granulating temperature to be 102 ℃, controlling the granulating pressure to be 1.41MPa, cooling after granulating, and cooling to be 9 ℃ to obtain sodium bisulfide particles;
the spraying speed of the sodium hydrosulfide in the pretreated melt is 450mL/min, the spraying temperature of the sodium hydrosulfide in the pretreated melt is 142 ℃, and the diameter of a sodium hydrosulfide nozzle of the pretreated melt is 0.25mm;
the injection rate of the sodium hydrosulfide for nucleation is 60g/min.
Example 3
(1) Melt pretreatment
Filtering the melt sodium hydrosulfide by alumina ceramic, wherein the filtering pressure is 1.70MPa, the filtering temperature is 131 ℃, and the pretreated melt sodium hydrosulfide is obtained after filtering;
the concentration of the melt sodium hydrosulfide is 69wt%;
the alumina content of the alumina ceramic was 91.4wt% and the porosity was 83.6%.
(2) Spray thermal bonding granulation
a. Preparation of sodium hydrosulfide for nucleation
Spraying a polyvinyl alcohol aqueous solution on solid sodium hydrosulfide, controlling the spraying temperature of the polyvinyl alcohol aqueous solution to 67 ℃, controlling the spraying amount of the polyvinyl alcohol aqueous solution to be 1.8 weight percent of the solid sodium hydrosulfide per minute, controlling the temperature of the solid sodium hydrosulfide to be 91 ℃ during spraying, continuously stirring while spraying, ending stirring after spraying, heating the sprayed solid sodium hydrosulfide in a nitrogen atmosphere, controlling the heating temperature to be 103 ℃, controlling the heating time to be 175min, and crushing the solid sodium hydrosulfide to 30 mu m after heating to obtain sodium hydrosulfide for nucleation;
the mass ratio of the solid sodium hydrosulfide to the polyvinyl alcohol aqueous solution is 5:13;
the concentration of the polyvinyl alcohol in the polyvinyl alcohol aqueous solution is 0.4 weight percent, and the molecular weight of the polyvinyl alcohol is 65000;
in the solid sodium hydrosulfide, the content of sodium hydrosulfide is 72.5%, the content of crystal water is 24.4%, the content of iron is 0.00011%, and the content of sodium sulfide is 2.1%;
b. granulating
Spraying the pretreated melt sodium bisulfide and sodium bisulfide for nucleation into a granulating tower together, fully mixing the pretreated melt sodium bisulfide and the sodium bisulfide for nucleation, controlling the granulating temperature to be 107 ℃, controlling the granulating pressure to be 1.32MPa, cooling after granulating, and cooling to be 11 ℃ to obtain sodium bisulfide particles;
the spraying speed of the sodium hydrosulfide in the pretreated melt is 550mL/min, the spraying temperature of the sodium hydrosulfide in the pretreated melt is 131 ℃, and the diameter of a sodium hydrosulfide nozzle of the pretreated melt is 0.35mm;
the injection rate of the sodium hydrosulfide for nucleation is 70g/min.
Comparative example 1
Unlike example 1, the melt pretreatment step was omitted, and in the granulation step of spray thermal bonding granulation, granulation was performed using untreated melt sodium hydrosulfide instead of pretreated melt sodium hydrosulfide, and the rest steps were the same, and granulation was performed.
Comparative example 2
In contrast to example 1, in the spray thermal bonding granulation step, sodium hydrosulfide for nucleation was prepared by the following procedure:
crushing solid sodium hydrosulfide to 25 mu m to obtain sodium hydrosulfide for nucleation;
in the solid sodium hydrosulfide, the content of sodium hydrosulfide is 72.5%, the content of crystal water is 24.4%, the content of iron is 0.00011%, and the content of sodium sulfide is 2.1%;
the rest steps are the same, and granulation is carried out.
Example 4 particle size detection
The granulation was carried out by the method of examples 1 to 3 and comparative examples 1 to 2, and the particle diameters of the obtained sodium hydrosulfide particles were measured and the respective ratios of the particle diameters of 0.2mm or less, 0.2 to 0.5mm, 0.5 to 1.0mm, 1.0 to 1.5mm and 1.5mm or more were counted, and the results are shown in Table 1.
TABLE 1
| Group of | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 |
| 0.2mm or less | 3.57% | 3.38% | 3.51% | 6.31% | 8.25% |
| 0.2-0.5mm | 11.62% | 10.96% | 12.07% | 15.67% | 6.57% |
| 0.5-1.0mm | 78.25% | 79.03% | 78.60% | 65.82% | 59.24% |
| 1.0-1.5mm | 5.34% | 4.85% | 4.73% | 9.58% | 15.94% |
| 1.5mm or more | 1.22% | 1.78% | 1.09% | 2.62% | 10.00% |
Examples 1-3 used melt pretreatment and prepared sodium hydrosulfide for nucleation as a nucleating agent, and further granulated, the obtained sodium hydrosulfide particles had a relatively concentrated particle size distribution, most of which were within 0.5-1.0 mm;
comparative example 1 omitted the melt pretreatment step, and the obtained sodium hydrosulfide particles had poor particle size concentration, although there was a large proportion of particles having a particle size within 0.5-1.0mm, the particles having a particle size within 0.2-0.5mm were too large, and the particles having other particle sizes were too large and were not concentrated in distribution;
in comparative example 2, untreated sodium bisulfide was used as a nucleating agent, and the obtained sodium bisulfide particles were poor in particle size concentration, only 59.24% of particles with particle sizes within 0.5-1.0mm were obtained, but more particles with particle sizes within 1.0-1.5mm were obtained, more particles with other particle sizes were obtained, and the distribution was most non-concentrated.
Example 5 moisture absorption test
Granulating by using the method of the embodiment 1-3 and the comparative example 1-2, performing moisture absorption performance test on the obtained sodium hydrosulfide particles, weighing 5g of sodium hydrosulfide particles into a weighing bottle, drying to constant weight, weighing after constant weight, putting the weighing bottle after constant weight into a constant temperature and humidity box which is stabilized to 25 ℃ and 80% RH, taking down a weighing bottle cap, putting the weighing bottle aside, closing a constant temperature and humidity box door, reaching a test end point after 3 hours, taking out the weighing bottle for weighing, performing blank comparison, calculating the moisture absorption percentage according to the following formula, counting, and observing whether the sodium hydrosulfide particles agglomerate or not after moisture absorption, wherein the result is shown in the table 2;
percentage of moisture uptake = [ (m 2-m 1) - (m 3-m 4) ]/(m 1-m 0) ×100
Wherein m2 is the mass of the sample and the weighing bottle after moisture absorption, and the unit is g;
m1 is the mass of the dried sample and the weighing bottle, and the unit is g;
m3 is the mass of the blank control moisture absorption empty weighing bottle, and the unit is g;
m4 is the mass of the empty weighing bottle before the blank control absorbs moisture, and the unit is g;
m0 is the mass of the weighing bottle, and the unit is g.
TABLE 2
| Group of | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 |
| Percentage of moisture absorption | 0.68% | 0.71% | 0.64% | 1.13% | 1.56% |
| Whether or not to agglomerate | Whether or not | Whether or not | Whether or not | Whether or not | The particles slightly aggregate |
Examples 1-3 used melt pretreatment and prepared sodium hydrosulfide for nucleation as a nucleating agent, and further granulated, the obtained sodium hydrosulfide particles have good moisture absorption resistance, and no caking is found after moisture absorption;
comparative example 1 omits the melt pretreatment step, and the obtained sodium hydrosulfide particles have slightly poorer moisture absorption capacity, but no caking is found after moisture absorption;
comparative example 2 used untreated sodium bisulfide as a nucleating agent, the resulting sodium bisulfide particles were less resistant to moisture absorption and slightly aggregated after moisture absorption.
Example 6 particle bubble detection
Pelletization was carried out by the method of examples 1-3 and comparative examples 1-2, and it was observed whether or not the obtained sodium bisulfide particles contained air bubbles, and the proportion of the sodium bisulfide particles containing air bubbles to the total was counted, and the results are shown in Table 3.
TABLE 3 Table 3
| Group of | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 |
| Sodium hydrosulfide particles containing air bubbles in total proportion | 2.58% | 2.31% | 2.46% | 7.29% | 11.34% |
Examples 1-3 used melt pretreatment and prepared sodium hydrosulfide for nucleation as a nucleating agent, and further granulated to obtain sodium hydrosulfide particles having a smaller proportion of bubbles inside;
comparative example 1 omits the melt pretreatment step, and the obtained sodium hydrosulfide particles have slightly higher proportion of bubbles in the interior;
comparative example 2 used untreated sodium hydrosulfide as a nucleating agent, and the obtained sodium hydrosulfide particles contained a higher proportion of bubbles inside.
Claims (7)
1. A method for granulating sodium hydrosulfide, which is characterized by comprising the steps of melt pretreatment, spray thermal bonding granulation;
the melt pretreatment method comprises the steps of filtering melt sodium hydrosulfide through alumina ceramic, wherein the filtering pressure is 1.60-1.70MPa, the filtering temperature is 131-142 ℃, and the pretreated melt sodium hydrosulfide is obtained after filtering;
the step of spray thermal bonding granulation comprises the steps of preparing sodium hydrosulfide for nucleation and granulating;
spraying a polyvinyl alcohol aqueous solution on solid sodium hydrosulfide, controlling the spraying temperature of the polyvinyl alcohol aqueous solution to be 63-67 ℃, controlling the spraying amount of the polyvinyl alcohol aqueous solution to be 1.8-2.1wt% of the solid sodium hydrosulfide per minute, controlling the temperature of the solid sodium hydrosulfide to be 84-91 ℃ during spraying, continuously stirring while spraying, ending stirring after spraying, heating the sprayed solid sodium hydrosulfide in a nitrogen atmosphere, controlling the heating temperature to be 92-103 ℃, controlling the heating time to be 175-210min, and crushing the solid sodium hydrosulfide to 20-30 mu m after heating to obtain the sodium hydrosulfide for nucleation;
the mass ratio of the solid sodium hydrosulfide to the polyvinyl alcohol aqueous solution is 5:11-13;
spraying pretreated melt sodium bisulfide and sodium bisulfide for nucleation into a granulating tower together, fully mixing the pretreated melt sodium bisulfide and the sodium bisulfide for nucleation, controlling the granulating temperature to be 102-107 ℃, controlling the granulating pressure to be 1.32-1.41MPa, and cooling after granulating to obtain sodium bisulfide particles;
the spraying speed of the sodium hydrosulfide in the pretreated melt is 450-550mL/min, and the spraying temperature of the sodium hydrosulfide in the pretreated melt is 131-142 ℃;
the spraying speed of the sodium hydrosulfide for nucleation is 60-70g/min.
2. A process for granulating sodium hydrosulfide according to claim 1, characterised in that:
in the melt pretreatment step, the concentration of the melt sodium hydrosulfide is 69-71wt%.
3. A process for granulating sodium hydrosulfide according to claim 1, characterised in that:
in the melt pretreatment step, the alumina content of the alumina ceramic was 91.4wt% and the porosity was 83.6%.
4. A process for granulating sodium hydrosulfide according to claim 1, characterised in that:
in the step of preparing sodium hydrosulfide for nucleation, the concentration of polyvinyl alcohol in the polyvinyl alcohol aqueous solution is 0.4-0.6wt% and the molecular weight of the polyvinyl alcohol is 53000-65000.
5. A process for granulating sodium hydrosulfide according to claim 1, characterised in that:
in the step of preparing sodium hydrosulfide for nucleation, in the solid sodium hydrosulfide, the content of sodium hydrosulfide is 72.5%, the content of crystal water is 24.4%, the content of iron is 0.00011%, and the content of sodium sulfide is 2.1%.
6. A process for granulating sodium hydrosulfide according to claim 1, characterised in that:
in the granulating step, the cooling temperature is 9-11 ℃.
7. A process for granulating sodium hydrosulfide according to claim 1, characterised in that:
in the granulating step, the diameter of a nozzle of the pretreated melt sodium hydrosulfide is 0.25-0.35mm.
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| CN115784169A (en) * | 2022-08-31 | 2023-03-14 | 平利县安得利新材料有限公司 | Purification method of sodium sulfide crystal |
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