CN108976176A - 3,3 '-diamino -4, the thinning method of 4 '-azoxy furazan explosive crystals - Google Patents
3,3 '-diamino -4, the thinning method of 4 '-azoxy furazan explosive crystals Download PDFInfo
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Abstract
本发明涉及含能材料领域，尤其是3，3’‑二氨基‑4,4’‑氧化偶氮呋咱炸药晶体的细化方法。该细化方法包括以下步骤：（1）将原料DAOAF与二甲基亚砜DMSO超声溶解后形成DAOAF溶液，并将DAOAF溶液倒入雾化喷头；（2）打开氮气加压，将DAOAF溶液经过雾化喷头形成小雾滴与非溶剂接触时，在超声搅拌的作用下迅速结晶析出DAOAF颗粒；（3）将DAOAF颗粒搅拌超声后过滤，并真空干燥；（4）采用激光粒度仪及扫描电子显微镜SEM对重结晶后的DAOAF进行进行粒度及形貌表征。本发明通过利用喷射反溶剂法快速脱除溶剂，同时利用搅拌及超声进一步打碎，更易实现DAOAF晶体颗粒的高效细化。细化后DAOAF在冲击片雷管用始发药、高能混合炸药及高能固体推进剂中将具有较好的发展前景。
The invention relates to the field of energetic materials, in particular to a method for refining 3,3'-diamino-4,4'-azofurazan explosive crystals. The refinement method includes the following steps: (1) ultrasonically dissolve the raw material DAOAF and dimethyl sulfoxide DMSO to form a DAOAF solution, and pour the DAOAF solution into the atomizing nozzle; (2) turn on the nitrogen and pressurize the DAOAF solution through When the atomizing nozzle forms small droplets and contacts with non-solvent, DAOAF particles are rapidly crystallized and precipitated under the action of ultrasonic stirring; (3) DAOAF particles are stirred ultrasonically, filtered, and dried in vacuum; (4) Laser particle size analyzer and scanning electron The particle size and morphology of recrystallized DAOAF were characterized by microscope SEM. In the present invention, the solvent is quickly removed by spraying the anti-solvent method, and at the same time, it is further broken by stirring and ultrasonic waves, so that the highly efficient refinement of DAOAF crystal particles can be more easily realized. After refinement, DAOAF will have a better development prospect in the starter charge for shock-disc detonators, high-energy mixed explosives and high-energy solid propellants.
Description
技术领域technical field
本发明涉及含能材料领域，尤其是3，3’-二氨基-4,4’-氧化偶氮呋咱炸药晶体的细化方法。The invention relates to the field of energetic materials, in particular to a method for refining the crystals of 3,3'-diamino-4,4'-azofurazan explosives.
背景技术Background technique
用于核武器的冲击片雷管是具有高性能、高安全的引爆工具。冲击片雷管用始发药应具有感度较低、使用性能好、起爆阈值低、爆轰能量高及热安定性好等特点。3,3'-二氨基-4,4'-氧化偶氮呋咱(DAOAF)是呋咱类炸药中典型代表物质。但DAOAF对撞击钝感，摩擦和静电火花不敏感。近年来，国内外对RDX(环三亚甲基/三硝胺，俗名黑索金)、HMX、HNS(六硝基苠)和TATB(三硝基-三胺基苯)等多种炸药进行形貌及粒度的控制。但至今国内外尚无关于DAOAF形貌及粒度控制的相关报道。Shock plate detonators used in nuclear weapons are detonating tools with high performance and high safety. The starting charge for shock plate detonators should have the characteristics of low sensitivity, good performance, low detonation threshold, high detonation energy and good thermal stability. 3,3'-Diamino-4,4'-azofurazan (DAOAF) is a typical representative of furazan explosives. But DAOAF is insensitive to impact insensitivity, friction and static sparks. In recent years, various explosives such as RDX (cyclotrimethylene/trinitramine, commonly known as RDX), HMX, HNS (hexanitrophenone) and TATB (trinitro-triaminobenzene) have been formed and developed at home and abroad. Appearance and granularity control. But so far there are no related reports on the morphology and particle size control of DAOAF at home and abroad.
发明内容Contents of the invention
本发明要解决的技术问题是：为了解决现有的DAOAF对撞击钝感，摩擦和静电火花不敏感的不足，本发明提供了一种3，3’-二氨基-4,4’-氧化偶氮呋咱炸药晶体的细化方法，通过利用喷射反溶剂法快速脱除溶剂，同时利用搅拌及超声进一步打碎，更易实现DAOAF晶体颗粒的高效细化。该方法操作简单，设备易获取，可通过不同操作获得不同粒径的DAOAF晶体，从而更好的控制获得DAOAF的不同粒径的晶体。细化后的DAOAF有较好的颗粒形态，粒径范围在500nm至1μm之间。晶体纯度大于99.6％。同时，DAOAF作为一种综合性能比较特别的含能材料。细化后DAOAF在冲击片雷管用始发药、高能混合炸药及高能固体推进剂中将具有较好的发展前景。The technical problem to be solved by the present invention is: in order to solve the existing DAOAF insensitivity to impact, friction and static spark insensitivity, the present invention provides a 3,3'-diamino-4,4'-oxo The refinement method of nitrogen furazan explosive crystals is to quickly remove the solvent by spraying anti-solvent method, and at the same time use stirring and ultrasonic to further break up, so that it is easier to achieve efficient refinement of DAOAF crystal particles. The method is simple to operate, and the equipment is easy to obtain. Different operations can be used to obtain DAOAF crystals with different particle sizes, so that the crystals with different particle sizes of DAOAF can be obtained under better control. The refined DAOAF has a better particle shape, and the particle size ranges from 500nm to 1μm. The crystal purity is greater than 99.6%. At the same time, DAOAF is an energetic material with special comprehensive properties. After refinement, DAOAF will have a better development prospect in the starter charge for shock-disc detonators, high-energy mixed explosives and high-energy solid propellants.
本发明解决其技术问题所采用的技术方案是：The technical solution adopted by the present invention to solve its technical problems is:
一种3，3’-二氨基-4,4’-氧化偶氮呋咱炸药晶体的细化方法，包括以下步骤：A method for refining 3,3'-diamino-4,4'-azofurazan explosive crystals, comprising the following steps:
(1)将原料DAOAF与二甲基亚砜DMSO超声溶解后形成DAOAF溶液，并将DAOAF溶液倒入雾化喷头；(1) The raw material DAOAF and DMSO are ultrasonically dissolved to form a DAOAF solution, and the DAOAF solution is poured into the atomizing nozzle;
(2)打开氮气加压，将DAOAF溶液经过雾化喷头形成小雾滴与非溶剂接触时，在超声搅拌的作用下迅速结晶析出DAOAF颗粒；(2) Turn on the nitrogen to pressurize, and when the DAOAF solution is passed through the atomizing nozzle to form small droplets and contact with the non-solvent, under the action of ultrasonic stirring, the DAOAF particles will be crystallized rapidly;
(3)将DAOAF颗粒搅拌超声后过滤，并真空干燥；(3) The DAOAF particles were stirred and ultrasonically filtered, and dried in vacuum;
(4)采用激光粒度仪及扫描电子显微镜SEM对重结晶后的DAOAF进行进行粒度及形貌表征。(4) The particle size and morphology of recrystallized DAOAF were characterized by laser particle size analyzer and scanning electron microscope SEM.
具体地，所述DAOAF溶液浓度为3％。Specifically, the concentration of the DAOAF solution is 3%.
具体地，所述雾化喷头口径为0.8mm或1mm或1.2mm。Specifically, the diameter of the atomizing nozzle is 0.8 mm or 1 mm or 1.2 mm.
具体地，所述氮气压强为0.4～0.6MPa。Specifically, the nitrogen pressure is 0.4-0.6 MPa.
具体地，所述DAOAF溶液与非溶剂的比例为1:40。Specifically, the ratio of the DAOAF solution to the non-solvent is 1:40.
具体地，所述非溶剂为去离子水。Specifically, the non-solvent is deionized water.
具体地，所述DAOAF溶液与非溶剂混合搅拌速度为450r/min。Specifically, the mixing speed of the DAOAF solution and the non-solvent is 450 r/min.
具体地，所述DAOAF溶液与非溶剂混合搅拌时间为45min，非溶剂温度为10摄氏度。Specifically, the mixing and stirring time of the DAOAF solution and the non-solvent is 45 minutes, and the temperature of the non-solvent is 10 degrees Celsius.
本发明的有益效果是：本发明提供了一种3，3’-二氨基-4,4’-氧化偶氮呋咱炸药晶体的细化方法，通过利用喷射反溶剂法快速脱除溶剂，同时利用搅拌及超声进一步打碎，更易实现DAOAF晶体颗粒的高效细化。该方法操作简单，设备易获取，可通过不同操作获得不同粒径的DAOAF晶体，从而更好的控制获得DAOAF的不同粒径的晶体。细化后的DAOAF有较好的颗粒形态，粒径范围在50nm至200nm之间。晶体纯度大于98.5％。同时，DAOAF作为一种综合性能比较特别的含能材料。细化后DAOAF在冲击片雷管用始发药、高能混合炸药及高能固体推进剂中将具有较好的发展前景。The beneficial effects of the present invention are: the present invention provides a method for refining 3,3'-diamino-4,4'-oxazofurazan explosive crystals, by using the spray anti-solvent method to quickly remove the solvent, and at the same time Using stirring and ultrasonic to further break up, it is easier to achieve efficient refinement of DAOAF crystal particles. The method is simple to operate, and the equipment is easy to obtain, and DAOAF crystals with different particle sizes can be obtained through different operations, so that the crystals with different particle sizes of DAOAF can be obtained under better control. The refined DAOAF has a better particle shape, and the particle size ranges from 50nm to 200nm. The crystal purity is greater than 98.5%. At the same time, DAOAF is an energetic material with special comprehensive properties. After refinement, DAOAF will have a better development prospect in the starter charge for shock-disc detonators, high-energy mixed explosives and high-energy solid propellants.
附图说明Description of drawings
下面结合附图和实施例对本发明进一步说明。The present invention will be further described below in conjunction with the accompanying drawings and embodiments.
图1是本发明的DAOAF原料颗粒分布图；Fig. 1 is the particle distribution figure of DAOAF raw material of the present invention;
图2是本发明的细化后DAOAF晶体的颗粒分布图；Fig. 2 is the particle distribution figure of DAOAF crystal after refinement of the present invention;
图3是本发明的细化后DAOAF的XRD图；Fig. 3 is the XRD figure of DAOAF after refinement of the present invention;
具体实施方式Detailed ways
现在结合附图对本发明作进一步详细的说明。The present invention is described in further detail now in conjunction with accompanying drawing.
图1是本发明的DAOAF原料颗粒分布图，图2是本发明的细化后DAOAF晶体的颗粒分布图，图3是本发明的细化后DAOAF的XRD图。Fig. 1 is a particle distribution diagram of the DAOAF raw material of the present invention, Fig. 2 is a particle distribution diagram of the refined DAOAF crystal of the present invention, and Fig. 3 is an XRD diagram of the refined DAOAF crystal of the present invention.
一种3，3’-二氨基-4,4’-氧化偶氮呋咱炸药晶体的细化方法，包括以下步骤：A method for refining 3,3'-diamino-4,4'-azofurazan explosive crystals, comprising the following steps:
(1)将原料DAOAF与二甲基亚砜DMSO超声溶解后形成DAOAF溶液，并将DAOAF溶液倒入雾化喷头；(1) The raw material DAOAF and DMSO are ultrasonically dissolved to form a DAOAF solution, and the DAOAF solution is poured into the atomizing nozzle;
(2)打开氮气加压，将DAOAF溶液经过雾化喷头形成小雾滴与非溶剂接触时，在超声搅拌的作用下迅速结晶析出DAOAF颗粒；(2) Turn on the nitrogen to pressurize, and when the DAOAF solution is passed through the atomizing nozzle to form small droplets and contact with the non-solvent, under the action of ultrasonic stirring, the DAOAF particles will be crystallized rapidly;
(3)将DAOAF颗粒搅拌超声后过滤，并真空干燥；(3) The DAOAF particles were stirred and ultrasonically filtered, and dried in vacuum;
(4)采用激光粒度仪及扫描电子显微镜SEM对重结晶后的DAOAF进行进行粒度及形貌表征。(4) The particle size and morphology of recrystallized DAOAF were characterized by laser particle size analyzer and scanning electron microscope SEM.
所述DAOAF溶液浓度为3％。所述雾化喷头口径为0.8mm或1mm或1.2mm。所述氮气压强为0.4～0.6MPa。所述DAOAF溶液与非溶剂的比例为1:40。所述非溶剂为去离子水。所述DAOAF溶液与非溶剂混合搅拌速度为450r/min。所述DAOAF溶液与非溶剂混合搅拌时间为45min，非溶剂温度为10摄氏度。The concentration of the DAOAF solution is 3%. The diameter of the atomizing nozzle is 0.8mm or 1mm or 1.2mm. The nitrogen pressure is 0.4-0.6 MPa. The ratio of the DAOAF solution to the non-solvent is 1:40. The non-solvent is deionized water. The mixing speed of the DAOAF solution and the non-solvent is 450 r/min. The mixing and stirring time of the DAOAF solution and the non-solvent is 45 minutes, and the temperature of the non-solvent is 10 degrees Celsius.
检测仪器：Testing equipment:
1.场发射扫描电镜；1. Field emission scanning electron microscope;
2.激光粒度仪；2. Laser particle size analyzer;
3.高效液相色谱仪。3. High performance liquid chromatography.
实施例一：Embodiment one:
首先将原料DAOAF溶于二甲基亚砜DMSO中，按照DAOAF(g)3:DMSO(ml)11的比例超声直至完全溶解成DAOAF溶液，并将DAOAF溶液倒入直径为0.8mm的雾化喷头。Firstly, dissolve the raw material DAOAF in dimethyl sulfoxide DMSO, ultrasonicate according to the ratio of DAOAF(g)3:DMSO(ml)11 until it is completely dissolved into a DAOAF solution, and pour the DAOAF solution into an atomizing nozzle with a diameter of 0.8mm .
然后打开氮气进行加压，压力值为0.6MPa,使DAOAF溶液经过雾化喷头形成小雾滴与非溶剂去离子水接触，迅速结晶析出DAOAF颗粒，同时超声并以450r/min的搅拌速度搅拌45min。最后过滤真空干燥。再利用激光粒度仪及SEM对重结晶后的DAOAF进行粒度及形貌表征。Then turn on the nitrogen to pressurize, the pressure value is 0.6MPa, make the DAOAF solution pass through the atomization nozzle to form small droplets and contact with non-solvent deionized water, and quickly crystallize and precipitate DAOAF particles, and at the same time, ultrasonic and stir at a stirring speed of 450r/min for 45min . Finally filter and dry in vacuo. The particle size and morphology of recrystallized DAOAF were characterized by laser particle size analyzer and SEM.
实施例二：Embodiment two:
首先将原料DAOAF与溶于二甲基亚砜DMSO中，按照DAOAF(g)3:DMSO(ml)11搅拌至完全溶解成DAOAF溶液，并将DAOAF溶液倒入直径为1mm的雾化喷头。First, dissolve the raw material DAOAF and DMSO in DMSO, stir according to DAOAF(g)3:DMSO(ml)11 until completely dissolved into a DAOAF solution, and pour the DAOAF solution into an atomizing nozzle with a diameter of 1mm.
然后打开氮气进行加压，压力值为0.6MPa,使DAOAF溶液经过雾化喷头形成雾滴与去离子水接触，超声并以450r/min的搅拌速度搅拌45min。最后结晶析出DAOAF颗粒并干燥。再利用扫描电镜、激光粒度分析等先进的仪器设备进行分析表征。Then turn on the nitrogen to pressurize, the pressure value is 0.6MPa, make the DAOAF solution pass through the atomization nozzle to form droplets and contact with deionized water, ultrasonic and stir at a stirring speed of 450r/min for 45min. Finally the DAOAF particles are crystallized out and dried. Then use scanning electron microscope, laser particle size analysis and other advanced equipment for analysis and characterization.
实施例二：Embodiment two:
首先将原料DAOAF与溶于二甲基亚砜DMSO中，按照DAOAF(g)3:DMSO(ml)11搅拌至完全溶解成DAOAF溶液，并将DAOAF溶液倒入直径为1.2mm的雾化喷头。First, dissolve the raw material DAOAF and DMSO in DMSO, stir according to DAOAF(g)3:DMSO(ml)11 until completely dissolved into a DAOAF solution, and pour the DAOAF solution into an atomizing nozzle with a diameter of 1.2mm.
然后打开氮气进行加压，压力值为0.6MPa,使DAOAF溶液经过雾化喷头形成雾滴与去离子水接触，超声并以450r/min的搅拌速度搅拌45min。最后结晶析出DAOAF颗粒并干燥。再利用扫描电镜、激光粒度分析等先进的仪器设备进行分析表征。Then turn on the nitrogen to pressurize, the pressure value is 0.6MPa, make the DAOAF solution pass through the atomization nozzle to form droplets and contact with deionized water, ultrasonic and stir at a stirring speed of 450r/min for 45min. Finally the DAOAF particles are crystallized out and dried. Then use scanning electron microscope, laser particle size analysis and other advanced equipment for analysis and characterization.
实施例四：Embodiment four:
首先将原料DAOAF与溶于二甲基亚砜DMSO中，按照DAOAF(g)3:DMSO(ml)11搅拌至完全溶解成DAOAF溶液，并将DAOAF溶液倒入直径为0.8mm的雾化喷头。First, dissolve the raw material DAOAF and DMSO in DMSO, stir according to DAOAF(g)3:DMSO(ml)11 until completely dissolved into a DAOAF solution, and pour the DAOAF solution into an atomizing nozzle with a diameter of 0.8mm.
然后打开氮气进行加压，压力值为0.4MPa,使DAOAF溶液经过雾化喷头形成雾滴与去离子水接触，超声并以450r/min的搅拌速度搅拌45min。最后结晶析出DAOAF颗粒并干燥。再利用扫描电镜、激光粒度分析等先进的仪器设备进行分析表征。Then turn on the nitrogen to pressurize, the pressure value is 0.4MPa, make the DAOAF solution pass through the atomization nozzle to form droplets and contact with deionized water, ultrasonic and stir at a stirring speed of 450r/min for 45min. Finally the DAOAF particles are crystallized out and dried. Then use scanning electron microscope, laser particle size analysis and other advanced equipment for analysis and characterization.
实施例五：Embodiment five:
首先将原料DAOAF与溶于二甲基亚砜DMSO中，按照DAOAF(g)3:DMSO(ml)11搅拌至完全溶解成DAOAF溶液，并将DAOAF溶液倒入直径为1mm的雾化喷头。First, dissolve the raw material DAOAF and DMSO in DMSO, stir according to DAOAF(g)3:DMSO(ml)11 until completely dissolved into a DAOAF solution, and pour the DAOAF solution into an atomizing nozzle with a diameter of 1mm.
然后打开氮气进行加压，压力值为0.4MPa,使DAOAF溶液经过雾化喷头形成雾滴与去离子水接触，超声并以450r/min的搅拌速度搅拌45min。最后结晶析出DAOAF颗粒并干燥。再利用扫描电镜、激光粒度分析等先进的仪器设备进行分析表征。Then turn on the nitrogen to pressurize, the pressure value is 0.4MPa, make the DAOAF solution pass through the atomization nozzle to form droplets and contact with deionized water, ultrasonic and stir at a stirring speed of 450r/min for 45min. Finally the DAOAF particles are crystallized out and dried. Then use scanning electron microscope, laser particle size analysis and other advanced equipment for analysis and characterization.
实施例六：Embodiment six:
首先将原料DAOAF与溶于二甲基亚砜DMSO中，按照DAOAF(g)3:DMSO(ml)11搅拌至完全溶解成DAOAF溶液，并将DAOAF溶液倒入直径为1.2mm的雾化喷头。First, dissolve the raw material DAOAF and DMSO in DMSO, stir according to DAOAF(g)3:DMSO(ml)11 until completely dissolved into a DAOAF solution, and pour the DAOAF solution into an atomizing nozzle with a diameter of 1.2mm.
然后打开氮气进行加压，压力值为0.6MPa,使DAOAF溶液经过雾化喷头形成雾滴与去离子水接触，超声并以450r/min的搅拌速度搅拌45min。最后结晶析出DAOAF颗粒并干燥。再利用扫描电镜、激光粒度分析等先进的仪器设备进行分析表征。Then turn on the nitrogen to pressurize, the pressure value is 0.6MPa, make the DAOAF solution pass through the atomization nozzle to form droplets and contact with deionized water, ultrasonic and stir at a stirring speed of 450r/min for 45min. Finally the DAOAF particles are crystallized out and dried. Then use scanning electron microscope, laser particle size analysis and other advanced equipment for analysis and characterization.
实施例七：Embodiment seven:
首先将原料DAOAF与溶于二甲基亚砜DMSO中，按照DAOAF(g)3:DMSO(ml)11搅拌至完全溶解成DAOAF溶液，并将DAOAF溶液倒入直径为0.8mm的雾化喷头。First, dissolve the raw material DAOAF and DMSO in DMSO, stir according to DAOAF(g)3:DMSO(ml)11 until completely dissolved into a DAOAF solution, and pour the DAOAF solution into an atomizing nozzle with a diameter of 0.8mm.
然后打开氮气进行加压，压力值为0.6MPa,使DAOAF溶液经过雾化喷头形成雾滴与去离子水接触，不使用超声的方式以450r/min的搅拌速度搅拌45min。最后结晶析出DAOAF颗粒并干燥。再利用扫描电镜、激光粒度分析等先进的仪器设备进行分析表征。Then turn on the nitrogen to pressurize, the pressure value is 0.6MPa, let the DAOAF solution pass through the atomization nozzle to form droplets and contact with deionized water, and stir at a stirring speed of 450r/min for 45min without using ultrasound. Finally the DAOAF particles are crystallized out and dried. Then use scanning electron microscope, laser particle size analysis and other advanced equipment for analysis and characterization.
实施例八：Embodiment eight:
首先将DAOAF与DMSO按照DAOAF(g)3:DMSO(ml)11的比例进行超声溶解后形成DAOAF溶液，并将DAOAF溶液倒入直径为0.8mm的雾化喷头。First, DAOAF and DMSO were ultrasonically dissolved according to the ratio of DAOAF(g)3:DMSO(ml)11 to form a DAOAF solution, and the DAOAF solution was poured into an atomizing nozzle with a diameter of 0.8mm.
然后打开氮气进行加压，压力值为0.6MPa,使DAOAF溶液经过雾化喷头形成雾滴与去离子水接触，只超声不搅拌.最后结晶析出DAOAF颗粒并干燥。再利用扫描电镜、激光粒度分析等先进的仪器设备进行分析表征。Then turn on the nitrogen to pressurize, the pressure value is 0.6MPa, make the DAOAF solution pass through the atomization nozzle to form droplets and contact with deionized water, only ultrasonic without stirring. Finally, DAOAF particles are crystallized and dried. Then use scanning electron microscope, laser particle size analysis and other advanced equipment for analysis and characterization.
实施例九：Embodiment nine:
首先将DAOAF与DMSO按照DAOAF(g)3:DMSO(ml)11的比例进行超声溶解后形成DAOAF溶液，并将DAOAF溶液倒入直径为0.8mm的雾化喷头。First, DAOAF and DMSO were ultrasonically dissolved according to the ratio of DAOAF(g)3:DMSO(ml)11 to form a DAOAF solution, and the DAOAF solution was poured into an atomizing nozzle with a diameter of 0.8mm.
然后打开氮气进行加压，压力值为0.6MPa,使DAOAF溶液经过雾化喷头形成雾滴与去离子水接触，超声并以50r/min的搅拌速度搅拌45min.最后结晶析出DAOAF颗粒并干燥。再利用扫描电镜、激光粒度分析等先进的仪器设备进行分析表征。Then turn on the nitrogen to pressurize, the pressure value is 0.6MPa, make the DAOAF solution pass through the atomization nozzle to form droplets and contact with deionized water, ultrasonic and stir at a stirring speed of 50r/min for 45min. Finally, DAOAF particles are crystallized and dried. Then use scanning electron microscope, laser particle size analysis and other advanced equipment for analysis and characterization.
实施例十：Embodiment ten:
首先将DAOAF与DMSO按照DAOAF(g)3:DMSO(ml)11的比例进行超声溶解后形成DAOAF溶液，并将DAOAF溶液倒入直径为0.8mm的雾化喷头。First, DAOAF and DMSO were ultrasonically dissolved according to the ratio of DAOAF(g)3:DMSO(ml)11 to form a DAOAF solution, and the DAOAF solution was poured into an atomizing nozzle with a diameter of 0.8mm.
然后打开氮气进行加压，压力值为0.6MPa,使DAOAF溶液经过雾化喷头形成雾滴与去离子水接触，超声并以200r/min的搅拌速度搅拌45min.最后结晶析出DAOAF颗粒并干燥。再利用扫描电镜、激光粒度分析等先进的仪器设备进行分析表征。Then turn on the nitrogen to pressurize, the pressure value is 0.6MPa, make the DAOAF solution pass through the atomization nozzle to form droplets and contact with deionized water, ultrasonic and stir at a stirring speed of 200r/min for 45min. Finally, DAOAF particles are crystallized and dried. Then use scanning electron microscope, laser particle size analysis and other advanced equipment for analysis and characterization.
实施例十一：Embodiment eleven:
首先将DAOAF与DMSO按照DAOAF(g)3:DMSO(ml)11的比例进行超声溶解后形成DAOAF溶液，并将DAOAF溶液倒入直径为0.8mm的雾化喷头。First, DAOAF and DMSO were ultrasonically dissolved according to the ratio of DAOAF(g)3:DMSO(ml)11 to form a DAOAF solution, and the DAOAF solution was poured into an atomizing nozzle with a diameter of 0.8mm.
然后打开氮气进行加压，压力值为0.6MPa,使DAOAF溶液经过雾化喷头形成雾滴与去离子水接触，超声并以450r/min的搅拌速度搅拌10min.最后结晶析出DAOAF颗粒并干燥。再利用扫描电镜、激光粒度分析等先进的仪器设备进行分析表征。Then turn on the nitrogen to pressurize, the pressure value is 0.6MPa, make the DAOAF solution pass through the atomizing nozzle to form droplets and contact with deionized water, ultrasonic and stir at a stirring speed of 450r/min for 10min. Finally, DAOAF particles are crystallized and dried. Then use scanning electron microscope, laser particle size analysis and other advanced equipment for analysis and characterization.
以上述依据本发明的理想实施例为启示，通过上述的说明内容，相关工作人员完全可以在不偏离本项发明技术思想的范围内，进行多样的变更以及修改。本项发明的技术性范围并不局限于说明书上的内容，必须要根据权利要求范围来确定其技术性范围。Inspired by the above-mentioned ideal embodiment according to the present invention, through the above-mentioned description content, relevant workers can make various changes and modifications within the scope of not departing from the technical idea of the present invention. The technical scope of the present invention is not limited to the content in the specification, but must be determined according to the scope of the claims.
本发明采用实施例1的方法制得细化后DAOAF晶体颗粒的形貌图与DAOAF原料相比。原料DAOAF晶体颗粒大小分布不均且形态均不统一，细化后的DAOAF的晶体形貌发生了明显的改变。首先通过反溶剂法使得DAOAF重结晶，同时通过超声和搅拌的作用下晶体被打碎，形成颗粒分散均匀且形态较好的晶体颗粒。The present invention adopts the method of Example 1 to prepare the topography diagram of the refined DAOAF crystal particle and compare it with the DAOAF raw material. The raw material DAOAF crystal particle size distribution is uneven and the shape is not uniform, and the crystal morphology of the refined DAOAF has changed significantly. Firstly, the DAOAF was recrystallized by the anti-solvent method, and at the same time, the crystals were broken under the action of ultrasound and stirring to form crystal particles with uniform particle dispersion and good shape.
结合附图1及附图2所示，分别为原料DAOAF及细化后DAOAF晶体的颗粒分布图。从图中可以看出原料DAOAF颗粒晶体尺寸较大，平均粒径约在为182.528nm左右。而采用实施例1中的方法将DAOAF细化后得到的粒径明显变小，平均粒径约在为108.213nm左右。Combined with Figure 1 and Figure 2, they are the particle distribution diagrams of raw DAOAF and refined DAOAF crystals, respectively. It can be seen from the figure that the raw material DAOAF particle crystal size is relatively large, and the average particle size is about 182.528nm. However, the particle size obtained by refining the DAOAF by the method in Example 1 is obviously smaller, and the average particle size is about 108.213nm.
附图2及附图3分别表示原料DAOAF与细化后DAOAF的XRD图。从图中可以看出细化前后晶形一致。Accompanying drawing 2 and accompanying drawing 3 show the XRD pattern of raw material DAOAF and refined DAOAF respectively. It can be seen from the figure that the crystal shape is consistent before and after refinement.
采用高效液相色谱的方法对细化前后DAOAF晶体的化学纯度进行分析，分别为97.74％和97.35％。说明采用本方法细化的DAOAF晶体仍具有高的化学纯度。能够满足使用要求。The chemical purity of DAOAF crystals before and after refinement was analyzed by high performance liquid chromatography, and they were 97.74% and 97.35%, respectively. It shows that the DAOAF crystal refined by this method still has high chemical purity. Can meet the use requirements.
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