CN119370803A - A method for preparing fine-particle potassium perchlorate - Google Patents
A method for preparing fine-particle potassium perchlorate Download PDFInfo
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- CN119370803A CN119370803A CN202411951372.2A CN202411951372A CN119370803A CN 119370803 A CN119370803 A CN 119370803A CN 202411951372 A CN202411951372 A CN 202411951372A CN 119370803 A CN119370803 A CN 119370803A
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- oil phase
- microemulsion
- potassium perchlorate
- particle size
- fine
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- AXZAYXJCENRGIM-UHFFFAOYSA-J dipotassium;tetrabromoplatinum(2-) Chemical compound [K+].[K+].[Br-].[Br-].[Br-].[Br-].[Pt+2] AXZAYXJCENRGIM-UHFFFAOYSA-J 0.000 title claims abstract description 61
- 229910001487 potassium perchlorate Inorganic materials 0.000 title claims abstract description 61
- 239000010419 fine particle Substances 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims description 7
- 239000004530 micro-emulsion Substances 0.000 claims abstract description 56
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000002608 ionic liquid Substances 0.000 claims abstract description 31
- 238000002156 mixing Methods 0.000 claims abstract description 30
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 28
- 239000007864 aqueous solution Substances 0.000 claims abstract description 28
- 238000002360 preparation method Methods 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 15
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000001103 potassium chloride Substances 0.000 claims abstract description 14
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 14
- BAZAXWOYCMUHIX-UHFFFAOYSA-M sodium perchlorate Chemical compound [Na+].[O-]Cl(=O)(=O)=O BAZAXWOYCMUHIX-UHFFFAOYSA-M 0.000 claims abstract description 14
- 229910001488 sodium perchlorate Inorganic materials 0.000 claims abstract description 14
- 239000003999 initiator Substances 0.000 claims abstract description 5
- 150000003254 radicals Chemical class 0.000 claims abstract description 5
- 239000004094 surface-active agent Substances 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 4
- WIMBFQPYJQMSCP-UHFFFAOYSA-N (1,2,2,3,3,4,4,5,5,6,6-undecafluorocyclohexyl) 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC1(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C1(F)F WIMBFQPYJQMSCP-UHFFFAOYSA-N 0.000 claims description 18
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical group N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 15
- 229920001213 Polysorbate 20 Polymers 0.000 claims description 15
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 15
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 claims description 15
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 claims description 15
- 238000004519 manufacturing process Methods 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 239000011147 inorganic material Substances 0.000 abstract description 2
- OZGWOALFBHODRB-UHFFFAOYSA-N (1,2,2,3,3,4,4,5,5,6,6-undecafluorocyclohexyl)methyl prop-2-enoate Chemical compound FC1(F)C(F)(F)C(F)(F)C(F)(COC(=O)C=C)C(F)(F)C1(F)F OZGWOALFBHODRB-UHFFFAOYSA-N 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 81
- 239000012071 phase Substances 0.000 description 73
- 238000003756 stirring Methods 0.000 description 24
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- 239000006185 dispersion Substances 0.000 description 11
- 238000009826 distribution Methods 0.000 description 11
- 238000002347 injection Methods 0.000 description 11
- 239000007924 injection Substances 0.000 description 11
- 238000002386 leaching Methods 0.000 description 11
- 238000009210 therapy by ultrasound Methods 0.000 description 11
- 238000012360 testing method Methods 0.000 description 9
- 238000005259 measurement Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 5
- 230000035945 sensitivity Effects 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- 238000004880 explosion Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000012074 organic phase Substances 0.000 description 2
- -1 quaternary ammonium salt cations Chemical class 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 description 1
- 238000001291 vacuum drying Methods 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
- C01B11/00—Oxides or oxyacids of halogens; Salts thereof
- C01B11/16—Perchloric acid
- C01B11/18—Perchlorates
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Medicines Containing Antibodies Or Antigens For Use As Internal Diagnostic Agents (AREA)
Abstract
The invention relates to the field of inorganic materials, in particular to a preparation method of fine-particle potassium perchlorate, which comprises the steps of adding double-bond ionic liquid, (perfluorocyclohexyl) methyl acrylate, a free radical initiator, a surfactant and n-butyl alcohol into cyclohexane to obtain an oil phase, equally dividing the oil phase into two parts, respectively adding a potassium chloride aqueous solution and a sodium perchlorate aqueous solution into the oil phase to obtain a microemulsion A and a microemulsion B, mixing the microemulsion A and the microemulsion B for reaction, centrifuging, collecting a product, washing and drying.
Description
Technical Field
The invention relates to the field of inorganic materials, in particular to a preparation method of fine-particle potassium perchlorate.
Background
Potassium perchlorate is a strong oxidant, has the characteristics of high combustion temperature, high combustion speed, strong oxidability and the like, and is one of important raw materials in the production of fireworks and crackers. The potassium perchlorate is inevitably rubbed in the production, storage, transportation and use processes, so that combustion and explosion are easy to cause accidents, and the problem of how to improve the stability of the potassium perchlorate in the production, storage, transportation and use processes and reduce the accident risk is urgent to be solved.
Disclosure of Invention
Aiming at the technical problems, the invention provides a preparation method of fine-particle potassium perchlorate.
The technical scheme adopted is as follows:
the preparation method of the fine-particle potassium perchlorate comprises the following steps:
Adding double bond ionic liquid, (perfluorocyclohexyl) methacrylate, a free radical initiator, a surfactant and n-butyl alcohol into cyclohexane to obtain an oil phase, equally dividing the oil phase into two parts to obtain an oil phase A and an oil phase B, adding a potassium chloride aqueous solution into the oil phase A to obtain a microemulsion A, adding a sodium perchlorate aqueous solution into the oil phase B to obtain a microemulsion B, mixing the microemulsion A and the microemulsion B for reaction, centrifuging, collecting a product, washing and drying;
The structure of the double bond ionic liquid is as follows:
;
Wherein R is alkyl with the carbon number less than or equal to 4;
n is a positive integer greater than or equal to 5;
The mass ratio of the double bond ionic liquid to the (perfluorocyclohexyl) methacrylate is 1:0.1-1.
Further, R is butyl, and R is preferably n-butyl (-Bu).
Further, n is 5, 6, 7 or 8, and n is preferably 5.
Further, the surfactant is composed of Span80 and Tween 20.
Further, the mass ratio of Span80 to Tween20 is 1-4:1-4.
Further, the free radical initiator is azobisisobutyronitrile and/or azobisisoheptonitrile.
Further, the temperature of the mixing reaction is 35 to 45 ℃, and the temperature of the mixing reaction is preferably 40 ℃.
Further, the mixing reaction time is 1-10h.
The invention has the beneficial effects that the invention provides the preparation method of the fine-particle potassium perchlorate, double-bond ionic liquid and (perfluorocyclohexyl) methacrylate are added for copolymerization while the microemulsion method is used for preparing the potassium perchlorate, so that the size of the potassium perchlorate can be limited during nucleation and growth, the generated copolymer has quaternary ammonium salt cations, long-chain carboxyl anions and fluorine-containing chain segments, the excellent antifriction effect can be achieved, the friction force among potassium perchlorate particles is reduced, the edge effect is not easy to occur, the surface defects of the potassium perchlorate are reduced, hot spots are relatively difficult to form, the stability of the potassium perchlorate is improved, the friction sensitivity of the prepared potassium perchlorate is 0, the particle size is small, and the safety is high during production, transportation and storage.
Detailed Description
The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention. The technology not mentioned in the present invention refers to the prior art, and unless otherwise indicated, the following examples and comparative examples are parallel tests, employing the same processing steps and parameters.
Example 1:
a preparation method of fine-particle potassium perchlorate comprises the following steps:
Adding 1g of double bond ionic liquid, 0.1g of (perfluorocyclohexyl) methacrylate, 0.01g of azodiisobutyronitrile, 7.5g of span80, 7.5g of Tween20 and 40g of n-butanol into 500g of cyclohexane, stirring and uniformly mixing to obtain an oil phase, dividing the oil phase into two parts, namely an oil phase A and an oil phase B, respectively adding 100ml of 1.6mol/L potassium chloride aqueous solution and 100ml of 1.6mol/L sodium perchlorate aqueous solution into the oil phase A and the oil phase B, carrying out ultrasonic treatment for 30min to obtain a microemulsion A and a microemulsion B, mixing the microemulsion A and the microemulsion B, stirring at a rotation speed of 60r/min for reaction for 5h at 40 ℃, adding a proper amount of acetone for demulsification, centrifuging at a rotation speed of 2000r/min for 5min, collecting a product, leaching with cold water, and drying.
The potassium perchlorate prepared in this example was used as a sample, the sample was dispersed by a circulating dispersion sample injection system, the sample was subjected to particle size testing by a laser particle size distribution analyzer, and the change in the particle size of the potassium perchlorate was measured by using equivalent particle sizes (D10, D50, D90), resulting in a particle size D90 of 50.22 μm, a particle size D50 of 34.65 μm, and a particle size D10 of 19.04 μm.
The structure of the double bond ionic liquid is as follows:
;
the preparation method of the double bond ionic liquid comprises the following steps:
Placing 0.5mol of 4-vinylbenzene caproic acid and 0.55mol of sodium hydroxide into a round bottom flask, adding 1200 ml deionized water, vigorously stirring at 50 ℃ for 6 hours, adding 0.5mol of tetrabutylammonium bromide into the mixed solution, stirring for reaction for 12 hours, adding chloroform, extracting the product into an organic phase, separating to remove the water phase, washing the organic phase with deionized water for several times, removing the organic solvent by using a rotary evaporator, and placing the obtained product into a 50 ℃ vacuum drying box for drying 24: 24 h.
Example 2:
a preparation method of fine-particle potassium perchlorate comprises the following steps:
Adding 1g of double bond ionic liquid, 0.2g of (perfluorocyclohexyl) methacrylate, 0.01g of azodiisobutyronitrile, 7.5g of span80, 7.5g of Tween20 and 40g of n-butanol into 500g of cyclohexane, stirring and uniformly mixing to obtain an oil phase, dividing the oil phase into two parts, namely an oil phase A and an oil phase B, respectively adding 100ml of 1.6mol/L potassium chloride aqueous solution and 100ml of 1.6mol/L sodium perchlorate aqueous solution into the oil phase A and the oil phase B, carrying out ultrasonic treatment for 30min to obtain a microemulsion A and a microemulsion B, mixing the microemulsion A and the microemulsion B, stirring at a rotation speed of 60r/min for reaction for 5h at 40 ℃, adding a proper amount of acetone for demulsification, centrifuging at a rotation speed of 2000r/min for 5min, collecting a product, leaching with cold water, and drying.
The structure and preparation method of the double bond ionic liquid are the same as those of example 1.
The potassium perchlorate prepared in this example was used as a sample, the sample was dispersed by a circulating dispersion sample injection system, the sample was subjected to particle size measurement by a laser particle size distribution analyzer, and the change in the particle size of the potassium perchlorate was measured by using equivalent particle sizes (D10, D50, D90), to obtain a particle size D90 of 48.05. Mu.m, a particle size D50 of 33.17. Mu.m, and a particle size D10 of 18.52. Mu.m.
Example 3:
a preparation method of fine-particle potassium perchlorate comprises the following steps:
Adding 1g of double bond ionic liquid, 0.3g of (perfluorocyclohexyl) methacrylate, 0.01g of azodiisobutyronitrile, 7.5g of span80, 7.5g of Tween20 and 40g of n-butanol into 500g of cyclohexane, stirring and uniformly mixing to obtain an oil phase, dividing the oil phase into two parts, namely an oil phase A and an oil phase B, respectively adding 100ml of 1.6mol/L potassium chloride aqueous solution and 100ml of 1.6mol/L sodium perchlorate aqueous solution into the oil phase A and the oil phase B, carrying out ultrasonic treatment for 30min to obtain a microemulsion A and a microemulsion B, mixing the microemulsion A and the microemulsion B, stirring at a rotation speed of 60r/min for reaction for 5h at 40 ℃, adding a proper amount of acetone for demulsification, centrifuging at a rotation speed of 2000r/min for 5min, collecting a product, leaching with cold water, and drying.
The structure and preparation method of the double bond ionic liquid are the same as those of example 1.
The potassium perchlorate prepared in this example was used as a sample, the sample was dispersed by a circulating dispersion sample injection system, the sample was subjected to particle size measurement by a laser particle size distribution analyzer, and the change in the particle size of the potassium perchlorate was measured by using equivalent particle sizes (D10, D50, D90), to obtain a particle size D90 of 46.64 μm, a particle size D50 of 33.61 μm, and a particle size D10 of 17.73 μm.
Example 4:
a preparation method of fine-particle potassium perchlorate comprises the following steps:
Adding 1g of double bond ionic liquid, 0.4g of (perfluorocyclohexyl) methacrylate, 0.01g of azodiisobutyronitrile, 7.5g of span80, 7.5g of Tween20 and 40g of n-butanol into 500g of cyclohexane, stirring and uniformly mixing to obtain an oil phase, dividing the oil phase into two parts, namely an oil phase A and an oil phase B, respectively adding 100ml of 1.6mol/L potassium chloride aqueous solution and 100ml of 1.6mol/L sodium perchlorate aqueous solution into the oil phase A and the oil phase B, carrying out ultrasonic treatment for 30min to obtain a microemulsion A and a microemulsion B, mixing the microemulsion A and the microemulsion B, stirring at a rotation speed of 60r/min for reaction for 5h at 40 ℃, adding a proper amount of acetone for demulsification, centrifuging at a rotation speed of 2000r/min for 5min, collecting a product, leaching with cold water, and drying.
The structure and preparation method of the double bond ionic liquid are the same as those of example 1.
The potassium perchlorate prepared in this example was used as a sample, the sample was dispersed by a circulating dispersion sample injection system, the sample was subjected to particle size testing by a laser particle size distribution analyzer, and the change in the particle size of the potassium perchlorate was measured by using equivalent particle sizes (D10, D50, D90), resulting in a particle size D90 of 46.89 μm, a particle size D50 of 32.14 μm, and a particle size D10 of 17.06 μm.
Example 5:
a preparation method of fine-particle potassium perchlorate comprises the following steps:
Adding 1g of double bond ionic liquid, 0.5g of (perfluorocyclohexyl) methacrylate, 0.01g of azodiisobutyronitrile, 7.5g of span80, 7.5g of Tween20 and 40g of n-butanol into 500g of cyclohexane, stirring and uniformly mixing to obtain an oil phase, dividing the oil phase into two parts, namely an oil phase A and an oil phase B, respectively adding 100ml of 1.6mol/L potassium chloride aqueous solution and 100ml of 1.6mol/L sodium perchlorate aqueous solution into the oil phase A and the oil phase B, carrying out ultrasonic treatment for 30min to obtain a microemulsion A and a microemulsion B, mixing the microemulsion A and the microemulsion B, stirring at a rotation speed of 60r/min for reaction for 5h at 40 ℃, adding a proper amount of acetone for demulsification, centrifuging at a rotation speed of 2000r/min for 5min, collecting a product, leaching with cold water, and drying.
The structure and preparation method of the double bond ionic liquid are the same as those of example 1.
The potassium perchlorate prepared in this example was used as a sample, the sample was dispersed by a circulating dispersion sample injection system, the sample was subjected to particle size measurement by a laser particle size distribution analyzer, and the change in the particle size of the potassium perchlorate was measured by using equivalent particle sizes (D10, D50, D90), resulting in a particle size D90 of 48.66 μm, a particle size D50 of 33.05 μm, and a particle size D10 of 17.94 μm.
Example 6:
a preparation method of fine-particle potassium perchlorate comprises the following steps:
Adding 1g of double bond ionic liquid, 0.6g of (perfluorocyclohexyl) methacrylate, 0.01g of azodiisobutyronitrile, 7.5g of span80, 7.5g of Tween20 and 40g of n-butanol into 500g of cyclohexane, stirring and uniformly mixing to obtain an oil phase, dividing the oil phase into two parts, namely an oil phase A and an oil phase B, respectively adding 100ml of 1.6mol/L potassium chloride aqueous solution and 100ml of 1.6mol/L sodium perchlorate aqueous solution into the oil phase A and the oil phase B, carrying out ultrasonic treatment for 30min to obtain a microemulsion A and a microemulsion B, mixing the microemulsion A and the microemulsion B, stirring at a rotation speed of 60r/min for reaction for 5h at 40 ℃, adding a proper amount of acetone for demulsification, centrifuging at a rotation speed of 2000r/min for 5min, collecting a product, leaching with cold water, and drying.
The structure and preparation method of the double bond ionic liquid are the same as those of example 1.
The potassium perchlorate prepared in this example was used as a sample, the sample was dispersed by a circulating dispersion sample injection system, the sample was subjected to particle size measurement by a laser particle size distribution analyzer, and the change in the particle size of the potassium perchlorate was measured by using equivalent particle sizes (D10, D50, D90), to obtain a particle size D90 of 49.27 μm, a particle size D50 of 34.30 μm, and a particle size D10 of 18.82 μm.
Example 7:
a preparation method of fine-particle potassium perchlorate comprises the following steps:
Adding 1g of double bond ionic liquid, 0.7g of (perfluorocyclohexyl) methacrylate, 0.01g of azodiisobutyronitrile, 7.5g of span80, 7.5g of Tween20 and 40g of n-butanol into 500g of cyclohexane, stirring and uniformly mixing to obtain an oil phase, dividing the oil phase into two parts, namely an oil phase A and an oil phase B, respectively adding 100ml of 1.6mol/L potassium chloride aqueous solution and 100ml of 1.6mol/L sodium perchlorate aqueous solution into the oil phase A and the oil phase B, carrying out ultrasonic treatment for 30min to obtain a microemulsion A and a microemulsion B, mixing the microemulsion A and the microemulsion B, stirring at a rotation speed of 60r/min for reaction for 5h at 40 ℃, adding a proper amount of acetone for demulsification, centrifuging at a rotation speed of 2000r/min for 5min, collecting a product, leaching with cold water, and drying.
The structure and preparation method of the double bond ionic liquid are the same as those of example 1.
The potassium perchlorate prepared in this example was used as a sample, the sample was dispersed by a circulating dispersion sample injection system, the sample was subjected to particle size measurement by a laser particle size distribution analyzer, and the change in the particle size of the potassium perchlorate was measured by using equivalent particle sizes (D10, D50, D90), resulting in a particle size D90 of 50.06 μm, a particle size D50 of 34.55 μm, and a particle size D10 of 19.10 μm.
Example 8:
a preparation method of fine-particle potassium perchlorate comprises the following steps:
Adding 1g of double bond ionic liquid, 0.8g of (perfluorocyclohexyl) methacrylate, 0.01g of azodiisobutyronitrile, 7.5g of span80, 7.5g of Tween20 and 40g of n-butanol into 500g of cyclohexane, stirring and uniformly mixing to obtain an oil phase, dividing the oil phase into two parts, namely an oil phase A and an oil phase B, respectively adding 100ml of 1.6mol/L potassium chloride aqueous solution and 100ml of 1.6mol/L sodium perchlorate aqueous solution into the oil phase A and the oil phase B, carrying out ultrasonic treatment for 30min to obtain a microemulsion A and a microemulsion B, mixing the microemulsion A and the microemulsion B, stirring at a rotation speed of 60r/min for reaction for 5h at 40 ℃, adding a proper amount of acetone for demulsification, centrifuging at a rotation speed of 2000r/min for 5min, collecting a product, leaching with cold water, and drying.
The structure and preparation method of the double bond ionic liquid are the same as those of example 1.
The potassium perchlorate prepared in this example was used as a sample, the sample was dispersed by a circulating dispersion sample injection system, the sample was subjected to particle size measurement by a laser particle size distribution analyzer, and the change in the particle size of the potassium perchlorate was measured by using equivalent particle sizes (D10, D50, D90), to obtain a particle size D90 of 50.80 μm, a particle size D50 of 35.12 μm, and a particle size D10 of 19.94 μm.
Example 9:
a preparation method of fine-particle potassium perchlorate comprises the following steps:
adding 1g of double bond ionic liquid, 0.9g of (perfluorocyclohexyl) methacrylate, 0.01g of azodiisobutyronitrile, 7.5g of span80, 7.5g of Tween20 and 40g of n-butanol into 500g of cyclohexane, stirring and uniformly mixing to obtain an oil phase, dividing the oil phase into two parts, namely an oil phase A and an oil phase B, respectively adding 100ml of 1.6mol/L potassium chloride aqueous solution and 100ml of 1.6mol/L sodium perchlorate aqueous solution into the oil phase A and the oil phase B, carrying out ultrasonic treatment for 30min to obtain a microemulsion A and a microemulsion B, mixing the microemulsion A and the microemulsion B, stirring at a rotation speed of 60r/min for reaction for 5h at 40 ℃, adding a proper amount of acetone for demulsification, centrifuging at a rotation speed of 2000r/min for 5min, collecting a product, leaching with cold water, and drying.
The structure and preparation method of the double bond ionic liquid are the same as those of example 1.
The potassium perchlorate prepared in this example was used as a sample, the sample was dispersed by a circulating dispersion sample injection system, the sample was subjected to particle size measurement by a laser particle size distribution analyzer, and the change in the particle size of the potassium perchlorate was measured by using equivalent particle sizes (D10, D50, D90), to obtain a particle size D90 of 51.25 μm, a particle size D50 of 35.09 μm, and a particle size D10 of 21.45 μm.
Example 10:
a preparation method of fine-particle potassium perchlorate comprises the following steps:
Adding 1g of double bond ionic liquid, 1g of (perfluorocyclohexyl) methacrylate, 0.01g of azodiisobutyronitrile, 7.5g of span80, 7.5g of Tween20 and 40g of n-butanol into 500g of cyclohexane, stirring and uniformly mixing to obtain an oil phase, dividing the oil phase into two parts, namely an oil phase A and an oil phase B, respectively adding 100ml of 1.6mol/L potassium chloride aqueous solution and 100ml of 1.6mol/L sodium perchlorate aqueous solution into the oil phase A and the oil phase B, carrying out ultrasonic treatment for 30min to obtain a microemulsion A and a microemulsion B, mixing the microemulsion A and the microemulsion B, stirring at a rotating speed of 60r/min for reaction for 5h at 40 ℃, adding a proper amount of acetone for demulsification, centrifuging at a rotating speed of 2000r/min for 5min, collecting a product, leaching with cold water, and drying.
The structure and preparation method of the double bond ionic liquid are the same as those of example 1.
The potassium perchlorate prepared in this example was used as a sample, the sample was dispersed by a circulating dispersion sample injection system, the sample was subjected to particle size measurement by a laser particle size distribution analyzer, and the change in the particle size of the potassium perchlorate was measured by using equivalent particle sizes (D10, D50, D90), to obtain a particle size D90 of 55.35 μm, a particle size D50 of 36.12 μm, and a particle size D10 of 22.01 μm.
Comparative example 1:
substantially the same as in example 1, except that (perfluorocyclohexyl) methacrylate was not added.
A preparation method of fine-particle potassium perchlorate comprises the following steps:
Adding 1g of double bond ionic liquid, 0.01g of azodiisobutyronitrile, 7.5g of span80, 7.5g of Tween20 and 40g of n-butanol into 500g of cyclohexane, stirring and uniformly mixing to obtain an oil phase, dividing the oil phase into two parts, namely an oil phase A and an oil phase B, respectively adding 100ml of 1.6mol/L aqueous solution of potassium chloride and 100ml of 1.6mol/L aqueous solution of sodium perchlorate into the oil phase A and the oil phase B, carrying out ultrasonic treatment for 30min to obtain a microemulsion A and a microemulsion B, mixing the microemulsion A and the microemulsion B, stirring at a rotation speed of 60r/min for reacting for 5h, adding a proper amount of acetone for demulsification, centrifuging at a rotation speed of 2000r/min for 5min, collecting a product, leaching with cold water, and drying.
The potassium perchlorate prepared in the comparative example is used as a sample, the sample is dispersed by a circulating dispersion sample injection system, the sample is subjected to particle size test by a laser particle size distribution instrument, and the change of the particle size of the potassium perchlorate is measured by adopting equivalent particle sizes (D10, D50 and D90), so that the particle size D90 is 60.06 mu m, the particle size D50 is 40.69 mu m and the particle size D10 is 25.58 mu m.
Performance test the potassium perchlorate prepared in examples 1 to 10 according to the invention and comparative example 1 was used as test specimen.
According to GJB 5891.24-2006 standard, the testing conditions are 90 degrees, 3.92MPa,20mg sample quantity, pendulum mass of (1500+ -1) g, environment temperature of (20+ -5) DEG C and relative humidity of 50-65%, one of the phenomena of sample discoloration, smell, smoke, explosion sound or ablation trace on the surface of a hit column in the test is judged to be exploded, otherwise, the test is judged to be unexplosive, each group of samples is parallelly tested for 25 times, and the testing result is expressed by explosion percentage;
;
As is clear from Table 1, the friction sensitivity of the potassium perchlorate prepared by the method is 0, and the safety is high in the production, transportation and storage processes.
As is clear from comparison of examples 1 to 10, when the mass ratio of the double bond ionic liquid to the (perfluorocyclohexyl) methacrylate is 1:0.1-1, the prepared potassium perchlorate is not only 0 in friction sensitivity, but also has smaller particle size;
as is clear from the comparison of example 1 and comparative example 1, the friction sensitivity of the prepared potassium perchlorate increased to 12% without adding (perfluorocyclohexyl) methacrylate, and the particle size was slightly increased.
The foregoing embodiments are merely for illustrating the technical solution of the present invention, but not for limiting the same, and although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those skilled in the art that modifications may be made to the technical solution described in the foregoing embodiments or equivalents may be substituted for parts of the technical features thereof, and that such modifications or substitutions do not depart from the spirit and scope of the technical solution of the embodiments of the present invention in essence.
Claims (8)
1. The preparation method of the fine-particle potassium perchlorate is characterized by comprising the following steps of:
Adding double bond ionic liquid, (perfluorocyclohexyl) methacrylate, a free radical initiator, a surfactant and n-butyl alcohol into cyclohexane to obtain an oil phase, equally dividing the oil phase into two parts to obtain an oil phase A and an oil phase B, adding a potassium chloride aqueous solution into the oil phase A to obtain a microemulsion A, adding a sodium perchlorate aqueous solution into the oil phase B to obtain a microemulsion B, mixing the microemulsion A and the microemulsion B for reaction, centrifuging, collecting a product, washing and drying;
The structure of the double bond ionic liquid is as follows:
;
Wherein R is alkyl with the carbon number less than or equal to 4;
n is a positive integer greater than or equal to 5;
The mass ratio of the double bond ionic liquid to the (perfluorocyclohexyl) methacrylate is 1:0.1-1.
2. The method for producing fine-grained potassium perchlorate according to claim 1, wherein R is butyl.
3. The method for producing fine-grained potassium perchlorate according to claim 1, wherein n is 5, 6, 7 or 8.
4. The method for preparing the fine-grained potassium perchlorate according to claim 1, wherein the surfactant consists of Span80 and Tween 20.
5. The method for preparing the fine-grained potassium perchlorate according to claim 4, wherein the mass ratio of Span80 to Tween20 is 1-4:1-4.
6. The method for producing fine-particle potassium perchlorate as claimed in claim 1, wherein the radical initiator is azobisisobutyronitrile and/or azobisisoheptonitrile.
7. The method for producing fine-grained potassium perchlorate according to claim 1, wherein the temperature of the mixing reaction is 35 to 45 ℃.
8. The method for producing fine-grained potassium perchlorate according to claim 1, wherein the time for the mixing reaction is 1 to 10 hours.
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