阅读说明：本技术 一种双氧水和磷酸联合改性活性炭电极材料的方法 (A kind of method of hydrogen peroxide and the combined modified active carbon electrode material of phosphoric acid ) 是由 张忠洁 宋文妹 陈鹏鹏 毛昌杰 吴明元 于 2019-09-20 设计创作，主要内容包括：一种双氧水和磷酸联合改性活性炭电极材料的方法,包括以下步骤：(1)活性炭预处理；(2)共振声混合；(3)超声波催化双氧水改性活性炭反应；(4)双氧水和磷酸处理；(5)清洗和干燥。本发明先用超声波催化质量分数为30%的双氧水改性纳米级活性炭,形成中孔；然后在形成中孔的基础上,再用双氧水和磷酸复合改性纳米级活性炭,进一步丰富活性炭表面的官能团,在碳材料表面形成-OH、-CHO等含氧官能团。(A kind of method of hydrogen peroxide and the combined modified active carbon electrode material of phosphoric acid, comprising the following steps: (1) Activated Carbon Pretreatment；(2) resonance sound mixes；(3) Catalyzed by Ultrasonic Wave hydrogen peroxide modified activated carbon reacts；(4) hydrogen peroxide and phosphoric acid processing；(5) it cleans and dry.It is 30% hydrogen peroxide modified Nano grade active carbon that the present invention, which first uses Catalyzed by Ultrasonic Wave mass fraction, forms mesoporous；Then on the basis of forming mesoporous, then with hydrogen peroxide and the composite modified nano level active charcoal of phosphoric acid, the functional group of activated carbon surface is further enriched, in oxygen-containing functional groups such as carbon material surface formation-OH ,-CHO.)

1. a kind of method of hydrogen peroxide and the combined modified active carbon electrode material of phosphoric acid, it is characterised in that: include the following steps:

Step 1: active carbon is crushed to 500-750nm, obtains nano level active charcoal, it is spare；

Step 2: nano level active charcoal and dehydrated alcohol being put into resonance sound mixer, in frequency 80-120Hz, amplitude 1.5- Under the conditions of 2.0mm, 240-360s is handled, mixture is obtained, it is spare；

Step 3: by hydrogen peroxide and mixture according to mass ratio 8-12:1, put into ultrasound reactor, at room temperature, with Ultrasonic frequency is 25-35KHz, power density 0.35-0.45w/cm², it is catalyzed reaction 30-35min, obtains the first reaction Object；

Step 4: the first reactant, hydrogen peroxide and phosphoric acid being mixed, are put into hydrothermal reaction kettle, closed hydrothermal reaction kettle, in temperature 5-7h is reacted at 59-61 DEG C of degree；

Step 5: the reaction mass that step 4 obtains being separated by solid-liquid separation, solid material is collected；Solids is cleaned with deionized water Material；Then it is dried, is ground into powdery after collecting dry solid material to get modified active carbon electrode material is arrived.

2. the method for hydrogen peroxide according to claim 1 and the combined modified active carbon electrode material of phosphoric acid, it is characterised in that: The active carbon is plant type active carbon, meets II grade of requirement, water content 5- in 37386 activated carbon for super capacitors of GB/T 7%, specific surface area 1500-1800m²/g。

3. the method for hydrogen peroxide according to claim 1 and the combined modified active carbon electrode material of phosphoric acid, it is characterised in that: The mass ratio of nano level active charcoal and dehydrated alcohol is 100:120-150.

4. the method for hydrogen peroxide according to claim 1 and the combined modified active carbon electrode material of phosphoric acid, it is characterised in that: Mass ratio between first reactant, hydrogen peroxide and phosphoric acid are as follows: 10:25-35:2-10.

5. the method for hydrogen peroxide according to claim 1 and the combined modified active carbon electrode material of phosphoric acid, it is characterised in that: The mass fraction of the phosphoric acid is 85-90%, and the mass fraction of hydrogen peroxide is 30%.

Technical field

The invention belongs to electrode material preparation technical field, it is related to a kind of hydrogen peroxide and the combined modified activated carbon electrodes of phosphoric acid The method of material.

Background technique

Supercapacitor refers to a kind of novel energy storage apparatus between traditional capacitor and rechargeable battery, it both had The characteristic of capacitor fast charging and discharging, while again with the energy storage characteristic of battery.Compared with battery and traditional physical capacitor, Supercapacitor has many advantages, such as that power density is high, has extended cycle life, the temperature that work limit for width, non-maintaining, environmentally protective.Super capacitor Device is the interfacial bilayer by being formed between electrode and electrolyte, carrys out fast storage and discharges the new component of charge.Electrode Material is one of the principal element for determining performance of the supercapacitor.

The type of supercapacitor can be divided into double layer capacitor, Faradic pseudo-capacitor (also referred to as by its working principle For fake capacitance capacitor) and the mixed capacitor that has concurrently of the two.Double layer capacitor is based on double electrode layer theory, using electrode and The interfacial electric double layer capacitor that is formed between electrolyte stores energy.Faradic pseudo-capacitor is then based on Faradaic processes, that is, exists It is generated during the electrochemical change of faraday's electric charge transfer, not only occurs on electrode surface, and electrode interior can be goed deep into. Therefore, whether the supercapacitor of which type, electrode material are all one of the principal elements for determining performance of the supercapacitor. According to both principles, be broadly divided into three classes currently as the electrode material of supercapacitor: carbon material, metal oxide and Hydrate material, conducting polymer materials.

Active carbon (AC) is the carbon electrode material that supercapacitor uses earliest, has low in cost, excellent conductivity, ratio The advantages that surface area is larger.But due to active carbon there are energy densities it is low, specific capacitance is smaller the disadvantages of, limit to a certain extent Its extensive use, it is modified need to carry out surface to it.Pore-size distribution, specific surface area, surface group are to determine absorbent charcoal material electricity An important factor for chemical property, therefore and the evaluation index of ruthenium ammonia synthesis catalyst effect.

Summary of the invention

The purpose of the present invention is to provide a kind of methods of hydrogen peroxide and the combined modified active carbon electrode material of phosphoric acid.

In order to achieve the above objects and other related objects, present invention provide the technical scheme that a kind of hydrogen peroxide and phosphoric acid The method of combined modified active carbon electrode material, including the following steps:

Step 1: active carbon is crushed to 500-750nm, obtains nano level active charcoal, it is spare；

Step 2: nano level active charcoal and dehydrated alcohol being put into resonance sound mixer, in frequency 80-120Hz, amplitude 1.5- Under the conditions of 2.0mm, 240-360s is handled, mixture is obtained, it is spare；

Step 3: by hydrogen peroxide and mixture according to mass ratio 8-12:1, put into ultrasound reactor, at room temperature, with Ultrasonic frequency is 25-35KHz, power density 0.35-0.45w/cm², it is catalyzed reaction 30-35min, obtains the first reaction Object；

Step 4: the first reactant, hydrogen peroxide and phosphoric acid being mixed, are put into hydrothermal reaction kettle, closed hydrothermal reaction kettle, in temperature 5-7h is reacted at 59-61 DEG C of degree；

Step 5: the reaction mass that step 4 obtains being separated by solid-liquid separation, solid material is collected；Solids is cleaned with deionized water Material；Then it is dried, is ground into powdery after collecting dry solid material to get modified active carbon electrode material is arrived.

Preferred technical solution are as follows: the active carbon is plant type active carbon, meets 37386 supercapacitor of GB/T use II grade of requirement, water content 5-7%, specific surface area 1500-1800m in active carbon²/g。

Preferred technical solution are as follows: the mass ratio of nano level active charcoal and dehydrated alcohol is 100:120-150.

Preferred technical solution are as follows: the mass ratio between the first reactant, hydrogen peroxide and phosphoric acid are as follows: 10:25-35:2- 10；

Preferred technical solution are as follows: the mass fraction of the phosphoric acid is 85-90%, and the mass fraction of hydrogen peroxide is 30%.

Since above-mentioned technical proposal is used, the present invention has the advantage, that compared with prior art

1, nano level active charcoal is efficiently uniformly mixed, significantly by the present invention by the way of resonance sound mixing with dehydrated alcohol Improve the rate and effect of successive modified reaction.

2, the hydrogen peroxide modified Nano grade active carbon that the present invention is first 30% with Catalyzed by Ultrasonic Wave mass fraction forms mesoporous； Then on the basis of forming mesoporous, then with hydrogen peroxide and the composite modified nano level active charcoal of phosphoric acid, active carbon is further enriched The functional group on surface, in oxygen-containing functional groups such as carbon material surface formation-OH ,-CHO.

3, the present invention uses hydrogen peroxide and the combined modified active carbon electrode material of phosphoric acid, the oxygen-containing official of modified activated carbon surface Can roll into a ball may generate fake capacitance by way of reversible redox reaction occurs, and greatly increase the ratio electricity of absorbent charcoal material Hold.

Detailed description of the invention

Fig. 1 modified active Carbon Materials are tested for the property, and detect the infrared spectrogram of AC-H60.

Fig. 2 uses cyclic voltammetry, with scanning voltage -1~0V, sweep speed 50mV/s, tests AC-0P electrode, AC-2P Electrode, AC-5P electrode, AC-8P electrode and AC-10P electrode obtain AC-0P electrode, AC-2P electrode, AC-5P electrode, AC-8P The CV curve of electrode and AC-10P electrode.

Specific embodiment

Embodiments of the present invention are illustrated by particular specific embodiment below, those skilled in the art can be by this explanation Content disclosed by book is understood other advantages and efficacy of the present invention easily.

Please refer to Fig. 1-2.It should be clear that this specification structure depicted in this specification institute accompanying drawings, ratio, size etc., only to match The revealed content of specification is closed, so that those skilled in the art understands and reads, is not intended to limit the invention implementable Qualifications, therefore do not have technical essential meaning, the modification of any structure, the change of proportionate relationship or the adjustment of size, In the case where not influencing the effect of present invention can be generated and the purpose that can reach, should all still fall in disclosed technology In the range of Rong get Neng is covered.Meanwhile it is cited such as "upper", "lower", "left", "right", " centre " and " one " in this specification Deng term, be merely convenient to being illustrated for narration, rather than to limit the scope of the invention, the change of relativeness Or adjustment, under the content of no substantial changes in technology, when being also considered as the enforceable scope of the present invention.