WO2020224101A1 - 一种包含氧化石墨烯的听性脑干刺激电极及其制作方法 - Google Patents

一种包含氧化石墨烯的听性脑干刺激电极及其制作方法 Download PDF

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WO2020224101A1
WO2020224101A1 PCT/CN2019/102222 CN2019102222W WO2020224101A1 WO 2020224101 A1 WO2020224101 A1 WO 2020224101A1 CN 2019102222 W CN2019102222 W CN 2019102222W WO 2020224101 A1 WO2020224101 A1 WO 2020224101A1
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electrode
graphene oxide
loop
oxide carrier
auditory brainstem
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French (fr)
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钱晓云
祁姝琪
高下
孙晓安
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浙江诺尔康神经电子科技股份有限公司
南京鼓楼医院
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61N—ELECTROTHERAPY; MAGNETOTHERAPY; RADIATION THERAPY; ULTRASOUND THERAPY
    • A61N1/00—Electrotherapy; Circuits therefor
    • A61N1/02—Details
    • A61N1/04—Electrodes
    • A61N1/0404—Electrodes for external use
    • A61N1/0472—Structure-related aspects
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61N—ELECTROTHERAPY; MAGNETOTHERAPY; RADIATION THERAPY; ULTRASOUND THERAPY
    • A61N1/00—Electrotherapy; Circuits therefor
    • A61N1/02—Details
    • A61N1/04—Electrodes
    • A61N1/05—Electrodes for implantation or insertion into the body, e.g. heart electrode
    • A61N1/0526—Head electrodes
    • A61N1/0529—Electrodes for brain stimulation
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61N—ELECTROTHERAPY; MAGNETOTHERAPY; RADIATION THERAPY; ULTRASOUND THERAPY
    • A61N1/00—Electrotherapy; Circuits therefor
    • A61N1/18—Applying electric currents by contact electrodes
    • A61N1/32—Applying electric currents by contact electrodes alternating or intermittent currents
    • A61N1/36—Applying electric currents by contact electrodes alternating or intermittent currents for stimulation
    • A61N1/3605—Implantable neurostimulators for stimulating central or peripheral nerve system
    • A61N1/3606—Implantable neurostimulators for stimulating central or peripheral nerve system adapted for a particular treatment
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61N—ELECTROTHERAPY; MAGNETOTHERAPY; RADIATION THERAPY; ULTRASOUND THERAPY
    • A61N1/00—Electrotherapy; Circuits therefor
    • A61N1/18—Applying electric currents by contact electrodes
    • A61N1/32—Applying electric currents by contact electrodes alternating or intermittent currents
    • A61N1/36—Applying electric currents by contact electrodes alternating or intermittent currents for stimulation
    • A61N1/3605—Implantable neurostimulators for stimulating central or peripheral nerve system
    • A61N1/36125—Details of circuitry or electric components
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
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    • C01B32/00—Carbon; Compounds thereof
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    • C01B32/198—Graphene oxide
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
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    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables

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  • the invention belongs to the field of medical devices, and particularly relates to an auditory brainstem stimulation electrode containing graphene oxide.
  • cochlear implant CI
  • cochlear nerve damage or complete loss of nerve function the lack of complete cochlear nerve function prevents the use of electronic cochlea to improve their hearing
  • auditory brainstem electrode implant ABSI is the lack of Designed for patients with complete cochlear nerve function.
  • Auditory brainstem implantation that is, after the electrodes are implanted into the cochlear nucleus of the brainstem, the sound signals are converted into electrical signals through the external receiver to stimulate the cochlear nerve to form an auditory pathway.
  • ABI is suitable for patients with neurofibromtosis type 2 (NF2), tympanic gasification, neurological deafness, and poor cochlear implantation. At present, there are about 100,000 such patients in my country, and the annual growth rate is about 6,000, so this new treatment technology is urgently needed.
  • the auditory brainstem implant directly acts on the brainstem, so the safety and sterility of the electrode carrier are higher.
  • the prior art generally uses medical silica gel, which only has a fixing effect.
  • the technical problem to be solved by the present invention is to provide a graphene oxide-containing auditory brain that can better contact the cochlear nucleus of the brainstem, has excellent antibacterial properties, promotes neuron growth, and has good biocompatibility. Dry stimulation electrodes.
  • an auditory brainstem stimulation electrode containing graphene oxide comprising a sheet loop electrode, a loop loop electrode, an electrode wire and a stimulation electrode arranged on a stimulator, wherein ,
  • the chip loop electrode is arranged on the stimulator, the stimulator is connected to a receiving coil, and an internal magnet is arranged on the receiving coil, which is connected to the external part of the auditory brainstem stimulation system by magnetic attraction;
  • the loop-type loop electrode is arranged one week outside the electrode wire coated with silica gel, close to the stimulator, and together with the sheet-type loop electrode, plays the role of a circuit loop when the stimulation electrode is stimulated;
  • One end of the electrode lead is connected to the stimulator; the other end is connected to the stimulation electrode;
  • the stimulation electrode includes a graphene oxide carrier, 19-24 electrode contacts, a first electrode fixing hole and a second electrode fixing hole, and the electrode contacts are arranged on the graphene oxide carrier and connected to each electrode wire.
  • An electrode fixing hole and a second electrode fixing hole are respectively arranged at both ends of the graphene oxide carrier.
  • the graphene oxide carrier includes a thin layer or powder of graphene oxide and an insulating material.
  • the electrode contact has a cap shape, and the bottom of the cap shape of the electrode contact exposes the graphene oxide carrier.
  • the present invention also provides a method for manufacturing an auditory brainstem stimulation electrode containing graphene oxide
  • the manufacturing method of graphene oxide thin layer or powder includes the following steps:
  • the centrifugal washing and drying in S37 includes the following steps:
  • the concentrated sulfuric acid concentration is 98%, and the concentrated phosphoric acid concentration is 85%.
  • potassium permanganate is added for 1 hour, and the temperature of the reaction system is 50 ⁇ 1°C.
  • the beneficial effects of the present invention are that the graphene oxide carrier of the auditory brainstem stimulation electrode containing graphene oxide can fit well with the brainstem cochlear nerve, graphene oxide can induce neuronal cell differentiation, and has excellent antibacterial properties. Compared with the use of medical silica gel in the prior art, it does not have the characteristics of the neural interface material of the present invention in terms of promoting the proliferation and transformation of neuronal cells and increasing the number of neurites, so as to ultimately achieve better recovery of hearing The effect of ability.
  • FIG. 1 is a schematic diagram of the implant structure of the auditory brainstem stimulation electrode containing graphene oxide according to the present invention
  • Figure 2 is an enlarged view of an auditory brainstem stimulation electrode containing graphene oxide according to the present invention
  • FIG. 3 is a schematic diagram of the application of the auditory brainstem stimulation electrode containing graphene oxide according to the present invention.
  • Fig. 4 is a flow chart of the steps of a method for manufacturing an auditory brainstem stimulation electrode containing graphene oxide of the present invention.
  • an auditory brainstem stimulation electrode containing graphene oxide includes a sheet loop electrode 3, a loop loop electrode 5, an electrode wire 6 and a stimulation electrode 8 arranged on a stimulator 4, wherein ,
  • the chip loop electrode 3 is arranged on the stimulator 4, the stimulator 4 is connected to the receiving coil 1, and the internal magnet 2 is arranged on the receiving coil 1, which is connected to the external part of the auditory brainstem stimulation system by magnetic suction;
  • the loop-type loop electrode 5 is arranged one week outside the silicone-coated electrode wire 6 and is close to the stimulator 4, and together with the sheet-type loop electrode 3, it functions as a circuit loop when the stimulation electrode 8 is stimulated;
  • One end of the electrode lead 6 is connected to the stimulator 4; the other end is connected to the stimulation electrode 8;
  • stimulating electricity, 8 includes graphene oxide carrier 8-1, 19-24 electrode contacts 8-2, first electrode fixing hole 8-3 and second electrode fixing hole 8-4, electrode contact 8 -2 is arranged on the graphene oxide carrier 8-1 to be connected to each electrode lead 6, and the first electrode fixing hole 8-3 and the second electrode fixing hole 8-4 are respectively arranged on both ends of the graphene oxide carrier 8-1 .
  • the graphene oxide carrier 8-1 includes a thin layer or powder of graphene oxide and an insulating material.
  • the electrode contact 8-2 has a cap shape, and the graphene oxide carrier 8-1 is exposed at the bottom of the cap shape of the electrode contact 8-2.
  • the present invention also provides a method for manufacturing an auditory brainstem stimulation electrode containing graphene oxide.
  • a flowchart of steps refer to FIG. 4,
  • the manufacturing method of graphene oxide thin layer or powder in S30 includes the following steps:
  • thermocouple temperature measurement device that comes with the oil bath is sometimes not very accurate, so add a thermometer in the oil bath; when adding potassium permanganate, it cannot be quickly added at one time. It will cause the temperature of the reaction system to increase sharply. To ensure that the temperature does not increase too quickly, potassium permanganate can be placed in a groove formed by folding a large filter paper, a small hole is cut at the bottom of the groove, and slowly dripped;
  • S36 Add diluted hydrogen peroxide to the mixture under heating and stirring at 50°C until the color of the solution changes from black to lavender to bright yellow, and no more bubbles; in order to prevent the temperature of the system from becoming due to the addition of hydrogen peroxide If it is too high, first dilute the hydrogen peroxide and then add it to the beaker, suck it with a syringe, then insert the syringe needle into the bottom of the reaction system and push the syringe slowly so that the temperature of the reaction system does not change too much. Adding hydrogen peroxide lasts about one hour, and the whole process reacts. The temperature of the system is maintained at 50 ⁇ 1°C.
  • Centrifugal washing and drying in S37 includes the following steps:
  • the concentration of concentrated sulfuric acid in S10 is 98%, and the concentration of concentrated phosphoric acid is 85%.
  • FIG. 3 is a schematic diagram of the application of an auditory brainstem stimulation electrode containing graphene oxide.
  • the stimulation electrode stimulates the dorsal nucleus of the cochlear nerve of the brainstem 11, together with the chip loop electrode 3 and the ring loop electrode 5. Form a circuit loop to complete effective electrical stimulation.

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Abstract

一种包含氧化石墨烯的听性脑干刺激电极及其制作方法，包括设置在刺激器（4）上的片式回路电极（3）、环式回路电极（5）、电极导线（6）和刺激电极（8），电极导线（6）一端与刺激器（4）连接；另一端与刺激电极（8）连接；刺激电极（8）包括氧化石墨烯载体（8-1）、19-24个电极触点（8-2）、第一电极固定孔（8-3）和第二电极固定孔（8-4）、电极触点（8-2）设置在氧化石墨烯载体（8-1）上与每根所述电极导线（6）连接，第一电极固定孔（8-3）和第二电极固定孔（8-4）分别设置在氧化石墨烯载体（8-1）的两端。氧化石墨烯载体（8-1）能更好地承担电极载体的功能，并诱导神经元细胞分化，还具备优异的抗菌性，达到更好的恢复听声能力的效果。

Description

一种包含氧化石墨烯的听性脑干刺激电极及其制作方法 技术领域
本发明属于医疗器械领域，特别涉及一种包含氧化石墨烯的听性脑干刺激电极。
背景技术
众所周知，深度耳聋的患者可以用植入电子耳蜗(cochlear implant，CI)的方法来改善听力。但是，对于那些耳蜗神经受损甚至神经功能完全丧失的患者，由于缺乏完整的蜗神经功能而无法通过电子耳蜗来改善其听力，听觉脑干电极植入(auditor brainstem plant，ABI)即为这些缺乏完整的蜗神经功能患者所设计。
听性脑干植入，即将电极植入脑干蜗核后，通过体外接收器讲声音信号转换成电信号刺激蜗神经从而形成听觉通路。ABI适用于2型神经纤维瘤病(neurofibromtosis type 2，NF2)、鼓室气化不良、神经性耳聋、植入人工耳蜗效果不佳等患者。目前我国此类患者约有10万人，且每年以约6000人的速度增长，所以迫切需要此项新的治疗技术。
听性脑干植入体直接作用于脑干，故对电极载体的安全性、无菌性要求更高，现有技术一般采用医用硅胶，仅具有固定作用。
发明内容
本发明要解决的技术问题是提供一种能更好地与脑干蜗神经核接触，具有 优异的抗菌性，促进神经元生长，具有良好的生物相容性的包含氧化石墨烯的听性脑干刺激电极。
为了实现上述目的，本发明的技术方案如下：一种包含氧化石墨烯的听性脑干刺激电极，包括设置在刺激器上的片式回路电极、环式回路电极、电极导线和刺激电极，其中，
所述片式回路电极设置在刺激器上，刺激器连接接收线圈，接收线圈上设置内磁体，与听性脑干刺激系统中的体外部分通过磁性吸力连接；
所述环式回路电极设置在硅胶包塑的所述电极导线外一周，靠近刺激器，与片式回路电极一同起到刺激电极刺激时的电路回路作用；
所述电极导线一端与刺激器连接；另一端与刺激电极连接；
所述刺激电极包括氧化石墨烯载体、19-24个电极触点、第一电极固定孔和第二电极固定孔、电极触点设置在氧化石墨烯载体上与每根所述电极导线连接，第一电极固定孔和第二电极固定孔分别设置在氧化石墨烯载体的两端。
优选地，所述氧化石墨烯载体包括氧化石墨烯薄层或粉末、绝缘材料。
优选地，所述电极触点为帽形，电极触点的帽形底部露出氧化石墨烯载体。
基于上述目的，本发明还提供了一种包含氧化石墨烯的听性脑干刺激电极的制作方法，
S10，对电极触点进行冲压和清洗，将电极导线与电极触点通过焊接相连；
S20，整理电极导线，将焊接电极触点的一端对齐，另一端将多余的电极导线剪掉；
S30，将调制好的氧化石墨烯薄层或粉末和绝缘材料的混合物注入模具一半深度，进行一次固化，在固化程度80％时，将电极触点交错排列，放入模具内；
S40，待混合物完全固化后，再将调制好的混合物注入模具，至电极触点没 过一半的深度，进行二次烘干固化，形成半包裹电极触点的氧化石墨烯载体；
S50，从模具中起模后，修剪多余氧化石墨烯载体，
其中，氧化石墨烯薄层或粉末的制作方法包括以下步骤：
S31，配制比例8∶1-9∶1的浓硫酸和浓磷酸的混酸200ml-300ml，放入干净干燥的烧杯中，待用；称取8g-12g高锰酸钾，待用；
S32，取1.5g-3g石墨置于反复洗刷干净干燥的500mL大烧杯中，将上述混酸缓慢沿杯壁倒入盛有石墨的烧杯中，待用；
S33，将油浴锅中加水，预热至50℃，再将上述混合反应物置于其中，用磁力搅拌器搅拌上述混合反应物；
S34，加入待用的高锰酸钾；
S35，将一张大滤纸盖住烧杯口，再将反应体系在50℃下加热6小时；
S36，在50℃加热和搅拌条件下向混合物中加入稀释后的双氧水，直到溶液颜色由黑色变成淡紫色到亮黄色，并不再产生气泡；
S37，将上述反应体系于50℃加热并搅拌3小时后，冷却至室温，进行离心洗涤及烘干。
优选地，所述S37中离心洗涤及烘干包括以下步骤：
S371，将冷却至室温的反应体系分到若干个烧杯中，分别加水稀释；
S372，将上述加水稀释后的反应物以9000rpm每次离心3-5min，pH值约等于6；
S373，在离心洗涤至少5次后，将得到的离心沉淀物稀释，存入棕色瓶或离心管中90℃下烘干为止。
优选地，所述浓硫酸浓度为98％，浓磷酸浓度为85％。
优选地，所述S34中，高锰酸钾加入持续1小时，反应体系温度为50±1℃。
本发明的有益效果在于：包含氧化石墨烯的听性脑干刺激电极的氧化石墨烯载体能与脑干蜗神经良好贴合，氧化石墨烯能够诱导神经元细胞分化，还具备优异的抗菌性，与现有技术中均采用医用硅胶相比，在促进神经元细胞的增 殖和转化，以及提升神经突的数量等方面不具备本发明的神经接口材料的特性，以最终达到更好的恢复听声能力的效果。
附图说明
图1为本发明包含氧化石墨烯的听性脑干刺激电极的植入体结构示意图；
图2为本发明包含氧化石墨烯的听性脑干刺激电极的放大图；
图3为本发明包含氧化石墨烯的听性脑干刺激电极的应用示意图；
图4为本发明包含氧化石墨烯的听性脑干刺激电极制作方法的步骤流程图。
具体实施方式
下面将结合附图，对本发明的优选实施例进行详细的描述。
参见图1-图3，一种包含氧化石墨烯的听性脑干刺激电极，包括设置在刺激器4上的片式回路电极3、环式回路电极5、电极导线6和刺激电极8，其中，
片式回路电极3设置在刺激器4上，刺激器4连接接收线圈1，接收线圈1上设置内磁体2，与听性脑干刺激系统中的体外部分通过磁性吸力连接；
环式回路电极5设置在硅胶包塑的电极导线6外一周，靠近刺激器4，与片式回路电极3一同起到刺激电极8刺激时的电路回路作用；
电极导线6一端与刺激器4连接；另一端与刺激电极8连接；
参见图2，刺激电，8包括氧化石墨烯载体8-1、19-24个电极触点8-2、第一电极固定孔8-3和第二电极固定孔8-4、电极触点8-2设置在氧化石墨烯载体8-1上与每根电极导线6连接，第一电极固定孔8-3和第二电极固定孔8-4分别设置在氧化石墨烯载体8-1的两端。
氧化石墨烯载体8-1包括氧化石墨烯薄层或粉末、绝缘材料。
电极触点8-2为帽形，电极触点8-2的帽形底部露出氧化石墨烯载体8-1。
与上述实施例对应的，本发明还提供了一种包含氧化石墨烯的听性脑干刺激电极的制作方法，步骤流程图参见图4，
S10，对电极触点进行冲压和清洗，将电极导线与电极触点通过焊接相连；
S20，整理电极导线，将焊接电极触点的一端对齐，另一端将多余的电极导线剪掉；
S30，将调制好的氧化石墨烯薄层或粉末和绝缘材料的混合物注入模具一半深度，进行一次固化，在固化程度80％时，将电极触点交错排列，放入模具内；
S40，待混合物完全固化后，再将调制好的混合物注入模具，至电极触点没过一半的深度，进行二次烘干固化，形成半包裹电极触点的氧化石墨烯载体；
S50，从模具中起模后，修剪多余氧化石墨烯载体，
其中，S30中氧化石墨烯薄层或粉末的制作方法包括以下步骤：
S31，配制比例8∶1-9∶1的浓硫酸和浓磷酸的混酸200ml-300mi，放入干净干燥的烧杯中，待用；称取8g-12g高锰酸钾，待用；
S32，取1.5g-3g石墨置于反复洗刷干净干燥的500mL大烧杯中，将上述混酸缓慢沿杯壁倒入盛有石墨的烧杯中，待用；
S33，将油浴锅中加水，预热至50℃，再将上述混合反应物置于其中，用磁力搅拌器搅拌上述混合反应物；
S34，加入待用的高锰酸钾；油浴锅自带的热电偶测温装置有时并不十分准确，故在油浴锅中加温度计；加入高锰酸钾时，不能一次快速加入，这样会使反应体系的温度急剧增加，为保证温度不至于增加太快，可把高锰酸钾放在一张大滤纸折叠成的凹槽中，在槽底剪一小洞，缓慢滴加；
S35，将一张大滤纸盖住烧杯口，再将反应体系在50℃下加热6小时；
S36，在50℃加热和搅拌条件下向混合物中加入稀释后的双氧水，直到溶液 颜色由黑色变成淡紫色到亮黄色，并不再产生气泡；为了使体系温度不至于因为加双氧水而变得太高，先把双氧水稀释再加入烧杯中，用注射器吸取，再把注射器针头插入反应体系的底部缓慢推注射器，使反应体系温度不至于变化太多，加双氧水持续时间约一个小时，整个过程反应体系温度维持在50±1℃。
S37，将上述反应体系于50℃加热并搅拌3小时后，冷却至室温，进行离心洗涤及烘干。
S37中离心洗涤及烘干包括以下步骤：
S371，将冷却至室温的反应体系分到若干个烧杯中，分别加水稀释；
S372，将上述加水稀释后的反应物以9000rpm每次离心3-5min，pH值约等于6；
S373，在离心洗涤至少5次后，将得到的离心沉淀物稀释，存入棕色瓶或离心管中90℃下烘干为止。
S10中浓硫酸浓度为98％，浓磷酸浓度为85％。
S34中，高锰酸钾加入持续1小时，反应体系温度为50±1℃。
在具体应用实施例中，参见图3，为包含氧化石墨烯的听性脑干刺激电极的应用示意图，刺激电极刺激脑干蜗神经背核11，与片式回路电极3和环式回路电极5形成电路回路，完成有效电刺激。
最后说明的是，以上优选实施例仅用以说明本发明的技术方案而非限制，尽管通过上述优选实施例已经对本发明进行了详细的描述，但本领域技术人员应当理解，可以在形式上和细节上对其作出各种各样的改变，而不偏离本发明权利要求书所限定的范围。

Claims (7)

  1. 一种包含氧化石墨烯的听性脑干刺激电极，其特征在于，包括设置在刺激器上的片式回路电极、环式回路电极、电极导线和刺激电极，其中，
    所述片式回路电极设置在刺激器上，刺激器连接接收线圈，接收线圈上设置内磁体，与听性脑干刺激系统中的体外部分通过磁性吸力连接；
    所述环式回路电极设置在硅胶包塑的所述电极导线外一周，靠近刺激器，与片式回路电极一同起到刺激电极刺激时的电路回路作用；
    所述电极导线一端与刺激器连接；另一端与刺激电极连接；
    所述刺激电极包括氧化石墨烯载体、19-24个电极触点、第一电极固定孔和第二电极固定孔、电极触点设置在氧化石墨烯载体上与每根所述电极导线连接，第一电极固定孔和第二电极固定孔分别设置在氧化石墨烯载体的两端。
  2. 根据权利要求1所述的包含氧化石墨烯的听性脑干刺激电极，其特征在于，所述氧化石墨烯载体包括氧化石墨烯薄层或粉末、绝缘材料。
  3. 根据权利要求1所述的包含氧化石墨烯的听性脑干刺激电极，其特征在于，所述电极触点为帽形，电极触点的帽形底部露出氧化石墨烯载体。
  4. 一种如权利要求1-3所述的包含氧化石墨烯的听性脑干刺激电极的制作方法，其特征在于，包括以下步骤：
    S10，对电极触点进行冲压和清洗，将电极导线与电极触点通过焊接相连；
    S20，整理电极导线，将焊接电极触点的一端对齐，另一端将多余的电极导线剪掉；
    S30，将调制好的氧化石墨烯薄层或粉末和绝缘材料的混合物注入模具一半深度，进行一次固化，在固化程度80％时，将电极触点交错排列，放入模具内；
    S40，待混合物完全固化后，再将调制好的混合物注入模具，至电极触点没过一半的深度，进行二次烘干固化，形成半包裹电极触点的氧化石墨烯载体；
    S50，从模具中起模后，修剪多余氧化石墨烯载体，
    其中，氧化石墨烯薄层或粉末的制作方法包括以下步骤：
    S31，配制比例8∶1-9∶1的浓硫酸和浓磷酸的混酸200ml-300ml，放入干净干燥的烧杯中，待用；称取8g-12g高锰酸钾，待用；
    S32，取1.5g-3g石墨置于反复洗刷干净干燥的500mL大烧杯中，将上述混酸缓慢沿杯壁倒入盛有石墨的烧杯中，待用；
    S33，将油浴锅中加水，预热至50℃，再将上述混合反应物置于其中，用磁力搅拌器搅拌上述混合反应物；
    S34，加入待用的高锰酸钾；
    S35，将一张大滤纸盖住烧杯口，再将反应体系在50℃下加热6小时；
    S36，在50℃加热和搅拌条件下向混合物中加入稀释后的双氧水，直到溶液颜色由黑色变成淡紫色到亮黄色，并不再产生气泡；
    S37，将上述反应体系于50℃加热并搅拌3小时后，冷却至室温，进行离心洗涤及烘干。
  5. 根据权利要求4所述的方法，其特征在于，所述S37中离心洗涤及烘干包括以下步骤：
    S371，将冷却至室温的反应体系分到若干个烧杯中，分别加水稀释；
    S372，将上述加水稀释后的反应物以9000rpm每次离心3-5min，pH值约等于6；
    S373，在离心洗涤至少5次后，将得到的离心沉淀物稀释，存入棕色瓶或离心管中90℃下烘干为止。
  6. 根据权利要求4所述的方法，其特征在于，所述浓硫酸浓度为98％，浓磷酸浓度为85％。
  7. 根据权利要求4所述的方法，其特征在于，所述S34中，高锰酸钾加入持续1小时，反应体系温度为50±1℃。
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