The invention relates to a.refractory materialThe preparation method belongs to the technical field of refractory material preparation. With the rapid development of science and technology, in order to prepare new materials with high temperature resistance, corrosion resistance, high performance and high efficiency, the refractory materials needed in the preparation process must be solved first. However, there are few oxide materials with high melting point, good chemical stability and excellent high temperature performance. With the rapid development of the iron and steel industry and the continuous improvement of the performance of electronic components, the application of refractory materials is more and more, in which the use of metallurgical industry is large, and the electronic industry is more distinctive. The refractory materials of metallurgical industry are mainly zircon sand for casting, and the nozzle basically adopts stable products. Refractory materials for electronic industry use the chemical stability and transformation toughening mechanism of materials.

Currentlyrefractory materialThe traditional production process is: 1. grading ingredients, dry mixing, pressing molding, drying, firing. The required pressure is high, causing great damage to equipment and molds. Semi-finished products are easy to cause demoulding damage, and the firing qualification rate is low. In addition, the firing temperature is relatively high. Secondly, the raw material powder is sprayed or granulated by a pair of rollers, pressed and molded, and then fired. The strength of the spherical particles obtained by spray granulation is low. Using double-roll granulation, the resulting particles are easy to break during the granulation process, and the yield is low; and the finished product has poor compactness, many pores, and uneven grain distribution. Generally speaking, refractory materials are difficult to sinter due to their high melting point, and the firing temperature should beMore than 1700.The firing temperature consumes a lot of energy, and the firing temperature range is narrow, which is easy to cause product cracking and deformation. In addition, there are a large number of pores in the dense part, resulting in poor thermal shock stability, and prone to explosion, cracking, and desolution during use.

The technical problem to be solved by the invention is.refractory materialDuring the preparation process, the product is easy to crack and deform, there are a large number of pores in the dense part, the thermal shock stability is poor, and the defects of cracking, cracking and dissolvability are easy to crack during use, The invention provides a preparation method for modified activated carbon, taking activated carbon and sulfuric acid solution insulation, ultrasonic oscillation to prepare modified activated carbon, stirring reaction with zirconium oxide, refrigeration, second static filtration, adding titanium dioxide, boron oxide and other mixed ball grinding, and then ball grinding. The preparation steps of the method are simple, the raw materials are easy to sinter, the energy consumption is low, the resulting product structure is dense and thermal shock stability is good, no cracking and deformation phenomenon, no cracking, cracking and desolation phenomenon during use.

In order to solve the above technical problems, the present invention adopts the following technical solutions:

(1) According to the solid-liquid ratio of 1:3, take 45% activated carbon and sulfuric acid solution into the container, then add 1.2-1.6 sodium dibutyl p-benzene disulfonate with -53khz mass fraction of activated carbon, then heat the container to 55-60, keep the temperature for 1-2h, naturally cool to room temperature, and put it into an ultrasonic oscillator with a set frequency of 48-53khz to oscillate for 45 minutes.

(2) 33-36 parts by weight of modified activated carbon, 22-25 parts by weight of zirconium oxychloride, 35-42 parts by weight of ethylene glycol, 9-13 parts by weight of dimethyl azelate, 6-8 parts by weight of urea and 2-4 parts by weight of lithium oxide are put into a high-pressure reaction kettle, protected by nitrogen, pressurized to 2-3 MPa, and heated.

(3) After the above reaction is over, depressurize to standard atmospheric pressure, naturally cool to 70-80, discharge while hot, place the discharge in a cold storage, let stand for 10-15 minutes from 0-5, then naturally heat to room temperature, filter, wash the filter residue with distilled water until neutral, and soak the washed filter residue with a mass fraction of 20%.

(4) Put 56-63 parts by weight of refractory substrate, 18-22 parts by weight of titanium dioxide, 11-13 parts by weight of boron oxide, 7-9 parts by weight of water, 5-7 parts by weight of iron oxide and 2-4 The weight of calcium lignosulfonate is placed in a ball mill and mixed for 20-30 minutes, and then placed in a mold to press and form a blank;

　　(5) Put the obtained blank into a drying oven, dry it at 100-115 for 8-10 hours, then put it into a calciner, protected by nitrogen, set the temperature at 1100-1300, heat preservation and sintering for 3-5 hours, and then Cool to room temperature with the furnace to getRefractory materials.

The present invention is prepared.refractory materialThe apparent porosity, density, compressive strength, flexural strength, fracture toughness and refractoriness were18.5-22.3%, 4.23-4.31g/m3, 308-342 MPa, 258-288 MPa, 2.5-2.8 MPa.

The thermal conductivity under 1000 and 825 is 3.70~3.72w/mk, the thermal shock resistance is 1000, and the water cooling is 18~20 times.

Compared with other methods, the beneficial technical effects of the present invention are:

(1) The preparation steps of the present invention are simple, the raw materials are easy to sinter, the energy consumption is small, the resulting product structure is good, no cracking and no deformation;(2) The thermal shock stability is good, and there is no explosion, cracking, and desolation during use.