CN110526224B - Mechanical ball milling synthesis method of phosphorus pentasulfide powder - Google Patents
Mechanical ball milling synthesis method of phosphorus pentasulfide powder Download PDFInfo
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- CN110526224B CN110526224B CN201910791155.4A CN201910791155A CN110526224B CN 110526224 B CN110526224 B CN 110526224B CN 201910791155 A CN201910791155 A CN 201910791155A CN 110526224 B CN110526224 B CN 110526224B
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- Prior art keywords
- ball milling
- powder
- phosphorus
- phosphorus pentachloride
- phosphorus pentasulfide
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- 238000000498 ball milling Methods 0.000 title claims abstract description 46
- 239000000843 powder Substances 0.000 title claims abstract description 33
- CYQAYERJWZKYML-UHFFFAOYSA-N phosphorus pentasulfide Chemical compound S1P(S2)(=S)SP3(=S)SP1(=S)SP2(=S)S3 CYQAYERJWZKYML-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000001308 synthesis method Methods 0.000 title claims abstract description 9
- UHZYTMXLRWXGPK-UHFFFAOYSA-N phosphorus pentachloride Chemical compound ClP(Cl)(Cl)(Cl)Cl UHZYTMXLRWXGPK-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000012265 solid product Substances 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- GLNWILHOFOBOFD-UHFFFAOYSA-N lithium sulfide Chemical compound [Li+].[Li+].[S-2] GLNWILHOFOBOFD-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000012298 atmosphere Substances 0.000 claims abstract description 8
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 39
- 239000007788 liquid Substances 0.000 claims description 19
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical group CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 239000007787 solid Substances 0.000 claims description 16
- 238000000926 separation method Methods 0.000 claims description 11
- 238000000227 grinding Methods 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 3
- 230000002194 synthesizing effect Effects 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000012300 argon atmosphere Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000002083 X-ray spectrum Methods 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- OBSZRRSYVTXPNB-UHFFFAOYSA-N tetraphosphorus Chemical compound P12P3P1P32 OBSZRRSYVTXPNB-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Classifications
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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
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/14—Sulfur, selenium, or tellurium compounds of phosphorus
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Secondary Cells (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a mechanical ball milling synthesis method of phosphorus pentasulfide powder, which comprises the following steps: (1) under the protection of inert atmosphere, adding phosphorus pentachloride and lithium sulfide powder into a sealed ball milling tank; (2) placing the ball milling tank on a ball mill at room temperature, and carrying out ball milling reaction at a certain rotating speed for a certain time; (3) after the reaction is finished, taking out the solid product from the ball milling tank in an inert atmosphere, and recovering the excessive phosphorus pentachloride; (4) and separating the residual solid product to obtain phosphorus pentasulfide powder. The preparation method of the phosphorus pentasulfide powder has the characteristics of simple process, low cost and easy industrial production.
Description
Technical Field
The invention belongs to the field of material synthesis, and relates to a mechanical ball-milling synthesis method of phosphorus pentasulfide powder.
Background
Phosphorus pentasulfide is an inorganic compound of the formula P2S5Yellow and yellowish green crystalline substances, which are stable when dried, but are easily hydrolyzed into phosphoric acid and hydrogen sulfide when meeting water. With the development of industries such as automobiles, petroleum, medicines and the like, the demand of high-quality phosphorus pentasulfide powder is increasing year by year. The existing synthetic method of phosphorus pentasulfide is mainly a liquid phase method (preparation method of Ligang, phosphorus pentasulfide), liquid elemental sulfur (sulfur) and phosphorus (yellow phosphorus) are fed into a reaction kettle according to the stoichiometric quantity for reaction, the obtained reaction product is distilled and purified, and then the purified liquid phosphorus pentasulfide is cooled and solidified. The existing synthesis process of phosphorus pentasulfide has the defects of complex preparation process, low quality of obtained products, high energy consumption and the likeTherefore, the development of a novel, efficient and environment-friendly synthetic method of phosphorus pentasulfide is of great significance.
Disclosure of Invention
The invention aims to solve the defects of the prior art and provides a novel method for synthesizing phosphorus pentasulfide powder, which is efficient, low in cost, environment-friendly and easy for industrial production.
The technical solution of the present invention is explained in detail below.
The invention relates to a mechanical ball milling synthesis method of phosphorus pentasulfide powder, which comprises the following steps:
(1) under the protection of inert atmosphere, adding phosphorus pentachloride and lithium sulfide powder into a sealed ball milling tank;
(2) the ball milling can is filled on a ball mill at room temperature, and mechanical ball milling reaction is carried out for a certain time at a certain rotating speed;
(3) after the reaction is finished, taking out the solid product from the ball milling tank in an inert atmosphere, and recovering the excessive phosphorus pentachloride;
(4) and adding the residual solid product into a certain amount of solvent, carrying out solid-liquid separation, and drying the solid to obtain phosphorus pentasulfide powder.
In the invention, the purity of the lithium sulfide powder and the phosphorus pentachloride is not lower than 90%.
In the invention, the molar ratio of the lithium sulfide powder to the phosphorus pentachloride in the step (1) is 5: (2-4).
In the invention, the ratio of the total mass of the lithium sulfide powder and the phosphorus pentachloride in the step (2) to the total mass of the grinding ball is 1: (10-80).
In the invention, in the step (2), the ball milling rotation speed is 100 and 500rpm/min, the ball milling time is 1-100h, and the mechanical ball milling reaction temperature is room temperature.
In the invention, in the step (3), the method for recovering the excessive phosphorus pentachloride comprises the steps of adding the solid product into toluene, carrying out solid-liquid separation to obtain a toluene solution containing the phosphorus pentachloride, and distilling the solution at the temperature of 110-.
In the invention, in the step (4), the solvent is acetone, and the addition amount of the acetone is based on the fact that impurities in the solid product are fully dissolved.
In the invention, in the step (4), the drying temperature is 80 ℃.
In the present invention, the inert atmosphere is a gas which does not react with lithium sulfide, phosphorus pentachloride, lithium chloride and phosphorus pentasulfide, such as argon, nitrogen or a mixed gas of nitrogen and argon.
In the invention, the room temperature is 0-40 ℃.
Compared with the prior art, the invention has the following beneficial effects:
the invention utilizes lithium sulfide and phosphorus pentachloride to synthesize phosphorus pentasulfide under mechanical ball milling, and is a green synthesis method with reasonable utilization of resources. The synthesis method has the advantages of high efficiency, low cost, environmental friendliness and easy industrial implementation.
Drawings
FIG. 1 is an X-ray diffraction pattern of a product synthesized in example 1 of the present invention.
Detailed description of the invention
The technical solution of the present invention is further described with reference to the following embodiments, but it should be noted that the scope of the present invention is not limited thereto.
The lithium sulfide powder and phosphorus pentachloride used in the examples of the present invention were not less pure than chemically pure (> 90%).
Example 1
Under the protection of argon atmosphere, 0.75g of lithium sulfide powder and 1.32g of phosphorus pentachloride are uniformly mixed and then added into a ball milling tank. Then the grinding balls are put into a ball milling tank and sealed. Wherein the ratio of the total mass of the grinding balls to the total mass of the materials is 40: 1. and (5) continuously performing ball milling reaction for 24 hours in a ball milling tank at the rotating speed of 500r/min at the room temperature. After the reaction is finished, taking out the solid product in the ball milling tank and adding the solid product into toluene in an argon atmosphere, carrying out solid-liquid separation, and distilling the separated solution at 150 ℃ to recover liquid toluene and solid phosphorus pentachloride. And adding the residual solid into acetone, carrying out solid-liquid separation, and drying the solid at the temperature of 80 ℃ to obtain phosphorus pentasulfide powder. FIG. 1 is an X-ray diffraction diagram of the product, which can only characterize the X-ray spectrum of lithium chloride, and phosphorus pentasulfide is contained in the product according to the law of element conservation.
Example 2
Under the protection of argon atmosphere, 1.78g of lithium sulfide powder and 4.9g of phosphorus pentachloride are uniformly mixed and then added into a ball milling tank. Then the grinding balls are put into a ball milling tank and sealed. Wherein the ratio of the total mass of the grinding balls to the total mass of the materials is 60: 1. and (5) continuously performing ball milling reaction for 100 hours in a ball milling tank at the rotating speed of 100r/min at the room temperature. After the reaction is finished, taking out the solid product in the ball milling tank and adding the solid product into toluene in an argon atmosphere, carrying out solid-liquid separation, and distilling the separated solution at 110 ℃ to recover liquid toluene and solid phosphorus pentachloride. Adding the rest solid into acetone, separating solid and liquid, and drying the solid at 80 deg.C to obtain phosphorus pentasulfide powder
Example 3
Under the protection of argon atmosphere, 0.37g of lithium sulfide powder and 1.3g of phosphorus pentachloride are uniformly mixed and then added into a ball milling tank. Then the grinding balls are put into a ball milling tank and sealed. Wherein the ratio of the total mass of the grinding balls to the total mass of the materials is 20: 1. and (3) continuously performing ball milling reaction on the ball milling tank for 100 hours at the rotating speed of 300r/min at the room temperature. After the reaction is finished, taking out the solid product in the ball milling tank and adding the solid product into toluene in an argon atmosphere, carrying out solid-liquid separation, and distilling the separated solution at 120 ℃ to recover liquid toluene and solid phosphorus pentachloride. And adding the residual solid into acetone, carrying out solid-liquid separation, and drying the solid at the temperature of 80 ℃ to obtain phosphorus pentasulfide powder.
Example 4
Under the protection of argon atmosphere, 0.71g of lithium sulfide powder and 1.29g of phosphorus pentachloride are uniformly mixed and then added into a ball milling tank. Then the grinding balls are put into a ball milling tank and sealed. Wherein the ratio of the total mass of the grinding balls to the total mass of the materials is 40: 1. and (5) continuously performing ball milling reaction for 1h in a ball milling tank at the rotating speed of 450r/min at the room temperature. After the reaction is finished, taking out the solid product in the ball milling tank and adding the solid product into toluene in an argon atmosphere, carrying out solid-liquid separation, and distilling the separated solution at 140 ℃ to recover liquid toluene and solid phosphorus pentachloride. And adding the residual solid into acetone, carrying out solid-liquid separation, and drying the solid at the temperature of 80 ℃ to obtain phosphorus pentasulfide powder.
Claims (5)
1. A mechanical ball milling synthesis method of phosphorus pentasulfide powder is characterized by comprising the following steps:
(1) under the protection of inert atmosphere, adding phosphorus pentachloride and lithium sulfide powder into a sealed ball milling tank;
(2) the ball milling can is filled on a ball mill at room temperature, and mechanical ball milling reaction is carried out for a certain time at a certain rotating speed;
(3) after the reaction is finished, taking the solid product out of the ball milling tank in an inert atmosphere to recover excessive phosphorus pentachloride;
(4) adding the residual solid product into a certain amount of solvent, carrying out solid-liquid separation, and drying the solid to obtain phosphorus pentasulfide powder;
wherein, the molar ratio of the lithium sulfide powder to the phosphorus pentachloride in the step (1) is 5: (2-4);
in the step (2), the ball milling rotation speed is 100-;
in the step (3), the method for recovering the excessive phosphorus pentachloride comprises the steps of adding the solid product into toluene, carrying out solid-liquid separation to obtain a toluene solution containing the phosphorus pentachloride, and distilling and recovering liquid toluene and solid phosphorus pentachloride at the temperature of 110-;
in the step (4), the solvent is acetone, and the addition amount of the acetone is based on the fact that impurities in the solid product are fully dissolved.
2. The method for synthesizing phosphorus pentasulfide powder by mechanical ball milling as claimed in claim 1, wherein the purity of lithium sulfide powder and phosphorus pentachloride is not less than 90%.
3. The mechanical ball-milling synthesis method of phosphorus pentasulfide powder according to claim 1, wherein the ratio of the total mass of lithium sulfide powder and phosphorus pentachloride in the step (2) to the total mass of the grinding balls is 1: (10-80).
4. The method for synthesizing phosphorus pentasulfide powder by mechanical ball milling as claimed in claim 1, wherein in the step (4), the drying temperature is 80 ℃.
5. The method as claimed in claim 1, wherein the inert atmosphere is a gas which does not react with lithium sulfide, phosphorus pentachloride, lithium chloride and phosphorus pentasulfide, and comprises argon, nitrogen and a mixture of nitrogen and argon.
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Patent Citations (10)
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