Method for preparing magnesium peroxide by high-energy rays

Abstract

The invention discloses a method for preparing magnesium peroxide by high-energy rays, which comprises the following steps of: fully and uniformly mixing magnesium oxide powder with a small amount of graphene, and then placing the mixed material in an irradiation environment of X-ray beams under the conditions that the voltage of a high-energy ray emitter is 30-40KV and the current of the high-energy ray emitter is 30-40mA, so that active sites are formed on magnesium oxide by excitation; under the condition that the irradiation condition of the X-ray light beam is kept unchanged, ozone is introduced, so that the ozone and active sites on the magnesium oxide are rapidly combined and react to generate peroxy bonds, synthesis of the magnesium peroxide is realized, and after the reaction is finished, discharging is performed to obtain a finished product of the magnesium peroxide. The process steps are simple and convenient, water is not introduced as a medium, the reaction is carried out in a gas phase environment, the links of solid-liquid separation, washing and drying are omitted, the reaction time is greatly saved, the content of magnesium peroxide in the product is high, and the product can be well applied in industry.

Description

Technical Field

[0001] The invention relates to a method for preparing magnesium peroxide with high-energy rays. Background Art

[0002] Magnesium peroxide is an important inorganic peroxide that is odorless, non-toxic, almost tasteless and has many excellent properties. Magnesium peroxide has important applications in environmental protection fields such as wastewater treatment and soil remediation. It can slowly release ozone in water and play a role in the degradation of organic pollutants. It can be used to decompose organic pollutants, reduce water pollution, and purify air and water sources.

[0003] The traditional method for synthesizing magnesium peroxide is to react hydrogen peroxide with magnesium oxide or magnesium chloride to produce magnesium peroxide. The magnesium oxide liquid phase method is a commonly used synthesis method. In a certain solution medium, magnesium peroxide is produced by reacting magnesium oxide with a hydrogen peroxide solution. The reaction temperature is controlled, and the finished magnesium peroxide is then dried. However, this method has the following technical drawbacks: 1. Complex process: The process requires a large amount of water as a medium. After the magnesium oxide is evenly dispersed, hydrogen peroxide is added. After the reaction is completed, solid-liquid separation is required, and the product is finally dried to obtain the product. Therefore, the post-processing step after the reaction is completed requires multiple steps of solid-liquid separation and drying.

[0004] 2. High cost: Since hydrogen peroxide releases a large amount of heat when reacting with magnesium peroxide liquid, if refrigerant is not added to cool it down, it will easily lead to decomposition and loss of hydrogen peroxide. Therefore, it is necessary to provide refrigerant to reduce the system temperature, which consumes a lot of energy.

[0005] 3. Low reaction conversion rate: The magnesium peroxide content is low, usually 25-35%. In actual application scenarios, a higher content is required to achieve ideal sterilization, oxygenation, and cleaning effects. The magnesium peroxide content prepared by high-energy rays can reach more than 40%. Summary of the Invention

[0006] In view of the above technical problems existing in the prior art, the object of the present invention is to provide a method for preparing magnesium peroxide using high-energy rays.

[0007] The technical solution adopted in the present invention is as follows: A method for preparing magnesium peroxide using high-energy rays comprises the following steps: S1 Magnesium oxide pretreatment: The reactor adopts a quartz kettle reactor, a rotary reactor or a spiral stirring reactor. Magnesium oxide powder is added to the reactor, and graphene with a mass fraction of 0.6-1% of magnesium oxide is added. Stir and mix to make the graphene and magnesium oxide fully mixed. Graphene with a large specific surface area can provide a good porous and loose reaction environment.

[0008] S2 irradiation treatment: Start the high-energy ray emitter to emit an X-ray beam, set the emitter voltage to 30-40 kV and the current to 30-40 mA, place the reactor in step S1 under the irradiation environment of the X-ray beam, and continuously stir the mixture in the reactor. X-rays pass through the reactor to irradiate the mixture therein. The high-energy rays excite the magnesium oxide ion crystals to generate hole-electron pairs. The high-energy rays gradually accumulate and produce a radiation displacement effect, which breaks or activates some magnesium-oxygen bonds in the magnesium oxide lattice, thereby forming highly active substances or hole sites within or on the surface of the magnesium oxide. In other words, active sites are excited to form on the magnesium oxide.

[0009] S3 ozone flow reaction: While maintaining the irradiation treatment conditions of step S2 unchanged, ozone is introduced into the reactor to rapidly combine with the active sites on the magnesium oxide to react and form peroxide bonds (-OO-), thereby achieving the synthesis of magnesium peroxide. After the reaction is completed, the finished magnesium peroxide is obtained by discharging the material.

[0010] Furthermore, in step S1, the kettle reactor is stirred by kettle stirring, the rotary reactor is stirred by reactor rotation, and the spiral stirring reactor is stirred by spiral stirring. For example, Chinese patent CN118179231A provides a spiral stirring reactor structure in its device structure, which can also achieve continuous feeding and discharging during the stirring process.

[0011] Furthermore, in step S1, the stirring speed is 30-60 r / min and the stirring time is 5-10 min.

[0012] Furthermore, the irradiation treatment time in step S2 is 10-20 minutes.

[0013] Furthermore, in step S2, the spherical reactor is driven to rotate at a speed of 80-120 r / min.

[0014] Furthermore, in step S3, the pressure of ozone in the reactor is from atmospheric pressure to a gauge pressure of 0.1 MPa.

[0015] Furthermore, the reaction time of step S3 is 30-60 min.

[0016] Furthermore, the reactor is made of ceramic, glass, quartz or other materials that can well transmit X-ray beams.

[0017] Compared with the prior art, the present invention has the following beneficial effects: 1) The process is simple: water is not introduced as a medium, and the reaction occurs in a gas phase environment, eliminating the solid-liquid separation, washing, and drying steps, greatly saving reaction time.

[0018] 2) Mild reaction: The temperature rise of the reaction system is very low under the action of high-energy rays, and no refrigerant is required for cooling, which saves energy consumption.

[0019] 3) High magnesium peroxide content in the product: This method has a high reaction conversion rate, stable products, low loss of active ingredients, and a high magnesium peroxide content in the product, reaching more than 40%. DETAILED DESCRIPTION

[0020] The present invention will be further described below with reference to specific embodiments, but the protection scope of the present invention is not limited thereto.

[0021] In the experiments of Examples 1-2 of the present invention, a glass flask was used as a tank reactor, and a stirring paddle was installed on the reactor for stirring. When ozone was required during the reaction, a balloon was tied to one opening of the glass flask, and ozone was introduced to inflate the balloon. This resulted in the ozone pressure within the reactor being close to 1 atmosphere, and the reaction was carried out under the ozone balloon pressure.

[0022] Example 1: 1. Magnesium oxide pretreatment: Prepare 40 g of magnesium oxide in advance and add it to a glass flask while adjusting the stirring speed to 30 r / min. Then add 0.3 g of graphene, plug the opening of the glass flask with a stopper and seal it. Continue stirring to ensure uniform mixing to provide a porous and loose reaction environment for the magnesium oxide. The mixing time is 5 minutes.

[0023] 2. Start the high-energy ray emitter: Start the high-energy ray emitter to emit X-ray beams, set the emitter voltage to 40kV, the current to 35mA, and increase the stirring speed to 80r / min. X-rays penetrate the glass flask and irradiate the mixture, ensuring that the high-energy X-rays fully and evenly contact the magnesium oxide mixture in the system. This process lasts for 10 minutes. The high-energy rays fully excite the magnesium oxide, forming active sites on the magnesium oxide, which empowers subsequent reactions.

[0024] 3. Ozone flow reaction: briefly stop the high-energy ray emitter, slowly introduce ozone into the glass flask to replace the air in the glass flask, then tie a balloon to one opening of the glass flask, inflate the balloon under the action of ozone, then stop introducing ozone, and then react under the pressure of the ozone balloon. According to the high-energy X-ray irradiation conditions in step 2, continue to emit X-ray beams. As the high-energy rays continue to irradiate, the magnesium oxide is further activated, and ozone quickly combines with the active sites on the magnesium oxide to form stable peroxide bonds, thereby realizing the synthesis of magnesium peroxide. The reaction time is 30 minutes. Afterwards, stop introducing ozone and the high-energy ray emitter, and discharge the material. The product mass is 45.67g, and the magnesium peroxide content is 41.15%.

[0025] Example 2: The experimental process of Example 2 is repeated in Example 1, except that: ① The amount of graphene added in step 1 is changed to 0.4g; ②In step 2, set the transmitter voltage to 40kV and the current to 30mA.

[0026] The final product mass of Example 2 was 45.77 g, and the magnesium peroxide content was 41.06%.

[0027] Comparative Example 1 (traditional process): 200 g of tap water was added to the reaction vessel as a base medium, and stirring was started at 100 r / min.

[0028] Add 40g of magnesium oxide to the reactor and stir evenly for 10 minutes.

[0029] Prepare 34 g of 35% hydrogen peroxide in advance and slowly add it to the system. Use a refrigerant to control the temperature of the reaction system at 20-30°C and the reaction time is 30 minutes.

[0030] After the reaction is completed, filter and wash with a suction flask for 30 minutes.

[0031] After filtration, the wet magnesium oxide is dried in an oven to obtain the finished product, which takes 30 minutes.

[0032] Summary: The reaction time was 100 min, the magnesium peroxide content was 35.2%, and the product mass was 44.48 g.

[0033] Comparative Example 2: The experimental process of Comparative Example 2 is repeated as in Example 1, with the only difference being that “the graphene in step 1 is replaced by silicon dioxide of the same mass”, and the other conditions remain unchanged.

[0034] The final product mass of Comparative Example 2 was 44.78 g, and the magnesium peroxide content was 35.02%.

[0035] The experimental results of Examples 1-2 and Comparative Examples 1-3 are compared in Table 1: .

[0036] 1. High-energy X-rays: High-energy X-rays are used to provide powerful excitation conditions for the reaction, causing magnesium oxide as an ionic crystal to undergo energy changes at the microscopic level. High-energy rays excite magnesium oxide ionic crystals to produce hole-electron pairs, which in turn produce a radiation displacement effect, breaking or activating the magnesium-oxygen bonds in the magnesium oxide lattice, thereby forming highly active substances or hole sites inside or on its surface.

[0037] 2. Ozone gas flow reaction: The reaction conditions provided by high-energy rays enable ozone to smoothly react with magnesium ions to form magnesium peroxide, forming a stable peroxide bond (-OO-).

[0038] 3. Graphene: Graphene has a very high specific surface area and provides a loose and porous environment for gas phase reactions.

[0039] The contents described in this specification are merely an enumeration of implementation forms of the inventive concept, and the protection scope of the present invention should not be considered as being limited to the specific forms described in the embodiments.

Claims

1. A method for preparing magnesium peroxide by high-energy rays, characterized in that The following steps are involved: S1 Magnesium oxide pretreatment: The reactor adopts a tank reactor, a rotary reactor or a spiral stirring reactor, adds magnesium oxide powder into the reactor, and adds graphene with a mass fraction of 0.6-1% of magnesium oxide, stirs and mixes, and makes the graphene and magnesium oxide fully mixed; S2 irradiation treatment: starting a high-energy ray emitter to emit an X-ray beam, setting the emitter voltage to 30-40 kV and the current to 30-40 mA, placing the reactor in step S1 under the irradiation environment of the X-ray beam, and continuously stirring the mixture in the reactor. X-rays penetrate the reactor to irradiate the mixture therein, thereby stimulating the formation of active sites on the magnesium oxide; S3 ozone flow reaction: while keeping the irradiation treatment conditions of step S2 unchanged, ozone is introduced into the reactor to rapidly combine with the active sites on the magnesium oxide to react and form peroxide bonds, thereby realizing the synthesis of magnesium peroxide. After the reaction is completed, the finished magnesium peroxide is obtained by discharging the material.

2. The method for preparing magnesium peroxide by high-energy rays according to claim 1, wherein In step S1, the stirring speed is 30-60 r / min and the stirring time is 5-10 min.

3. The method for preparing magnesium peroxide by high-energy rays according to claim 1, wherein The irradiation treatment time in step S2 is 10-20 minutes.

4. The method for preparing magnesium peroxide by high-energy rays according to claim 1, wherein In step S2, the stirring speed is 80-120 r / min.

5. The method for preparing magnesium peroxide by high-energy rays according to claim 1, wherein In step S3, the pressure of ozone in the reactor is from normal pressure to a gauge pressure of 0.1 MPa.

6. The method for preparing magnesium peroxide by high-energy rays according to claim 1, wherein The reaction time of step S3 is 30-60 min.

7. The method for preparing magnesium peroxide by high-energy rays according to claim 1, wherein The reactor is made of ceramic, glass or quartz.