CN109626554B - Preparation method of solid oxygen particles with oxygen slow-release function - Google Patents

Abstract

The invention discloses a preparation method of solid oxygen particles with a slow-release oxygen function, which is characterized in that clay and diatomite are calcined and ground and then are uniformly mixed with ferrous sulfate powder to obtain a mixture A; uniformly mixing percarbamide, potassium hydrogen persulfate powder and biochar, then mixing with a polyvinylpyrrolidone solution, stirring and uniformly dispersing to obtain a mixture B; and adding the mixture B into the mixture A, uniformly mixing to obtain a mixture C, and tabletting by adopting a rotary tablet press to obtain solid oxygen granules. The method has the advantages of simple operation, simple and nontoxic used reagents, wide application, strong practicability, capability of slowly generating oxygen for a long time and the like.

Description

Preparation method of solid oxygen particles with oxygen slow-release function

Technical Field

The invention relates to a preparation method of solid oxygen particles with an oxygen slow-release function, belonging to the field of preparation of solid oxygen materials.

Background

The general term "solid oxygen" refers to white or colored granular oxygen increasing agent made of sodium percarbonate, stabilizer and synergist, the oxygen increasing agent adopts special cylindrical granular design, can directly sink to the bottom of the pond, generates a large amount of oxygen after reacting with water, rapidly increases the dissolved oxygen in water, and can maintain the high dissolved oxygen in water for a period of time.

The existing black and odorous water body treatment technology can carry out aerobic treatment on organic matters in water to degrade and convert the organic matters into humus-like substances, but solid oxygen in the prior art cannot maintain a relatively stable dissolved oxygen concentration in the water body for a long time, so that the anaerobic environment mutates the aerobic environment, and aerobic microorganisms cannot be cultured in a short time.

In view of the requirement of providing a stable aerobic environment for the bottom of a river in aerobic biochemical treatment, it is important to obtain solid oxygen particles with a function of slowly releasing oxygen.

Disclosure of Invention

The invention aims to overcome the defects of the prior art and provides a preparation method of solid oxygen particles with an oxygen slow-release function. The method has the advantages of simple operation, single and easily obtained reagent, wide application and strong practicability, and can slowly generate oxygen for a long time.

The preparation method of the solid oxygen particles with the oxygen slow-release function comprises the following steps:

step 1: calcining and grinding clay and diatomite, and uniformly mixing the calcined and ground clay and ferrous sulfate powder to obtain a mixture A;

step 2: uniformly mixing percarbamide, potassium hydrogen persulfate powder and biochar, then mixing with a polyvinylpyrrolidone solution, stirring and uniformly dispersing to obtain a mixture B;

and step 3: and adding the mixture B into the mixture A, uniformly mixing to obtain a mixture C, and tabletting by adopting a rotary tablet press to obtain solid oxygen granules.

In the step 1, the calcining temperature is 300-500 ℃; the particle size after grinding is 0.1-1 mm.

In the step 1, the mass ratio of the clay, the diatomite and the ferrous sulfate is 0.1-0.5: 1: 0.15-0.6.

In the step 2, the mass ratio of percarbamide, potassium hydrogen persulfate and biochar is 1: 1: 0.1-0.6.

In the step 2, the addition mass of the polyvinylpyrrolidone solution is 2-5% of the mass of the mixture C, and the volume concentration of the polyvinylpyrrolidone solution is 0.5-5%.

In the step 3, the mixture A and the mixture B are mixed in a mass ratio of 1: 1.

Compared with the prior art, the invention has the beneficial effects that:

1. firstly, the mixture of percarbamide and potassium hydrogen persulfate is used as a releasing agent for the first time, so that the required released oxygen amount can be achieved, and the release is relatively stable; and secondly, polyvinylpyrrolidone is used as a slow-release cosolvent, so that the long-acting property of the release process is ensured.

2. The reagent adopted by the invention is nontoxic to water, can balance the pH of the water for a long time, and avoids large fluctuation of the pH value of the water. The biological carbon is used as a stabilizer, so that the stabilization effect of the particles in the water environment is ensured, and meanwhile, the biological carbon can adsorb organic pollutants in the water and promote the full contact of the pollutants and the generated oxygen.

3. The method for preparing the oxygen-release-delaying particles has the advantages of simple operation, single and easily obtained reagent, wide application, strong practicability, capability of slowly generating oxygen for a long time and the like, and has wide application prospect in black and odorous water treatment.

Drawings

FIG. 1 is a schematic representation of oxygen release in oxygen-free water for various amounts of solid oxygen particles. As can be seen from figure 1, the solid oxygen particles of the present invention can slowly release oxygen for a long time, and the amount of the oxygen-free water in 1L of the oxygen-free water is more than 6g, so that the oxygen-free water can be dissolved in about 5mg/L of oxygen for a long time.

FIG. 2 is a graphical representation of the change in pH of solid oxygen particles in oxygen-free water without the use of amounts of solid oxygen. As can be seen from FIG. 2, the solid oxygen particles of the present invention can slowly release oxygen compared to the mixture of percarbamide and oxone, and can balance the pH in water, and have a buffering effect on the pH value in water.

Detailed Description

The invention is further described below with reference to specific preferred embodiments, without thereby limiting the scope of protection of the invention.

The materials and equipment used in the following examples are commercially available.

Example 1: preparation of oxygen-extended particles

1. Preparing biochar through vacuum cracking, air-drying collected rice straws, grinding to enable the initial size to be smaller than 0.25mm, introducing nitrogen into a 350 ℃ tubular furnace for pyrolysis for 2 hours, sequentially washing the obtained biochar to be neutral by using 0.1mol/L HCl and ultrapure water, drying at 105 ℃, grinding, and filtering by using a 0.25mm screen to obtain the initial biochar material.

2. Calcining and grinding 0.2mg of clay and 1mg of diatomite at 500 ℃, and uniformly mixing with 0.3mg of ferrous sulfate powder to obtain a mixture A; uniformly mixing 1mg of percarbamide and potassium hydrogen persulfate powder and 0.2mg of charcoal in a mass ratio of 1:1, mixing with 0.3mg of polyvinylpyrrolidone solution (PVP, 3%) and fully stirring to obtain a mixture B; adding the mixture B into the mixture A, and tabletting by using a rotary tablet press to obtain the solid oxygen particles to be prepared.

Example 2:

1. 1L of boiled, sterilized and cooled distilled water is injected into a cylindrical reactor with the diameter of 10cm and the height of 15cm, a stirrer is arranged, and the reactor is sealed by a sealing plug. 0.2g of Na was put into the reactor from the drug inlet₂SO₃And 0.05gCoCl₂And closing the drug feeding port, removing dissolved oxygen in the reactor, and carrying out the next experiment when DO is reduced to 0mg/L and stabilized for 0.5 h.

2. Four reactors treated in the step 1 are placed on a workbench, 0g, 3g, 6g and 9g of the solid oxygen particles prepared in the example 1 are added into the four reactors respectively, and then a dissolved oxygen probe and a pH probe are inserted from a medicine inlet.

3. Dissolved oxygen and pH were measured in four reactors daily.

The solid oxygen particles can slowly release oxygen for a long time, and the dosage of more than 6g in 1L of oxygen-free water can ensure that the oxygen-free water is in the dissolved oxygen of about 5mg/L for a long time.

Example 3:

1. 1L of boiled, sterilized and cooled distilled water is injected into a cylindrical reactor with the diameter of 10cm and the height of 15cm, a stirrer is arranged, and the reactor is sealed by a sealing plug. 0.2g of Na was put into the reactor from the drug inlet₂SO₃And 0.05gCoCl₂Closing the drug feeding port, removing dissolved oxygen in the reactor, and when DO is reduced to 0mg/LAfter stabilizing for 0.5h, the next experiment can be carried out.

2. And (2) placing the three reactors treated in the step (1) on a workbench, respectively adding a mixture of 6g of solid oxygen particles, 6g of percarbamide and potassium hydrogen persulfate into the two reactors, not adding the other reactor as a blank group, and then inserting a pH value measuring probe and a dissolved oxygen probe from a medicine inlet.

3. The pH and dissolved oxygen in the three reactors were measured daily.

Compared with a mixture of percarbamide and potassium hydrogen persulfate, the solid oxygen particles can slowly release oxygen, can balance the pH value in water, and has a buffering effect on the pH value in the water body.

FIG. 1 is a schematic representation of oxygen release in oxygen-free water for various amounts of solid oxygen particles. As can be seen from the figure, the larger the amount of the solid oxygen pellets used, the higher the concentration of dissolved oxygen that can be achieved, and the higher the amount of the solid oxygen pellets used is by about 2mg/L, the higher the amount of the solid oxygen pellets used is by 6g, than the amount of the solid oxygen pellets used by 3g, but when the amount of the solid oxygen pellets used is 9g, the dissolved oxygen can be achieved by about 5.5mg/L at the beginning of the reaction, and after the reaction gradually stabilizes over time, the dissolved oxygen that can be achieved by about 5mg/L is almost the same as the dissolved oxygen concentration that can be achieved by 6 g. The dissolved oxygen in a 6g container of a mixture of percarbamide and oxone reached 7mg/L at 30h, after which a slow drop of 4mg/L at 120h was reached and also continued. It can be seen that the solid oxygen particles can slow down the oxygen release rate of the oxygen-releasing substance and can release oxygen efficiently for a long time so that the dissolved oxygen concentration is maintained at a high level.

FIG. 2 is a graphical representation of the change in pH of solid oxygen particles in oxygen-free water without the use of amounts of solid oxygen. As can be seen from the figure, the larger the amount of the solid oxygen particles used, the lower the pH of the solution, but the range of pH fluctuation was not so large that the basic pH was 6 or more and the pH was maintained in a stable state. The pH value dropped rapidly within the first 10h after the introduction of a 6g mixture of percarbamide and oxone, and finally stabilized at about 5. Therefore, the solid oxygen particles can balance the pH value in water and have a buffering effect on the pH value in the water body.

The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above-described embodiments. All technical schemes belonging to the idea of the invention belong to the protection scope of the invention. It should be noted that modifications and embellishments within the scope of the invention may be made by those skilled in the art without departing from the principle of the invention, and such modifications and embellishments should also be considered as within the scope of the invention.

Claims (3)

1. A preparation method of solid oxygen particles with a function of slowly releasing oxygen is characterized by comprising the following steps:

step 1: calcining and grinding clay and diatomite, and uniformly mixing the calcined and ground clay and ferrous sulfate powder to obtain a mixture A;

step 2: uniformly mixing percarbamide, potassium hydrogen persulfate powder and biochar, then mixing with a polyvinylpyrrolidone solution, stirring and uniformly dispersing to obtain a mixture B;

and step 3: adding the mixture B into the mixture A, uniformly mixing to obtain a mixture C, and tabletting by using a rotary tablet press to obtain solid oxygen particles;

in the step 1, the calcining temperature is 300-500 ℃;

in the step 1, the particle size after grinding is 0.1-1 mm;

in the step 1, the mass ratio of the clay, the diatomite and the ferrous sulfate is 0.1-0.5: 1: 0.15-0.6;

in the step 2, the mass ratio of percarbamide, potassium hydrogen persulfate and biochar is 1: 1: 0.1-0.6.

2. The method of claim 1, wherein:

in the step 2, the addition mass of the polyvinylpyrrolidone solution is 2-5% of the mass of the mixture C, and the volume concentration of the polyvinylpyrrolidone solution is 0.5-5%.

3. The method of claim 1, wherein:

in the step 3, the mixture A and the mixture B are mixed in a mass ratio of 1: 1.

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