CN104987086A - Fluoro-siloxane resin bonding carbon-rich fire resistant material and preparation method thereof - Google Patents

Abstract

The invention discloses a fluoro-siloxane resin bonding carbon-rich fire resistant material. The material is composed of, by weight, 10-12 parts of sisal fiber, 3-7 parts of fluoro-siloxane resin, 26-30 parts of tetraethoxysilane, 40-53 parts of crystalline flake graphite, 30-40 parts of amorphous graphite, 1-2 parts of octadecanoic acid, 0.7-2 parts of pentaerythritol, 0.1-0.17 part of benzotriazole, 3-4 parts of salpeter solutions of 10-13 mol/l, 2-3 parts of glacial acetic acid, 0.5-1 part of brown sugar, 2-3 parts of sodium potassium silicate and 6-8 parts of dimethyl carbonate. Under the condition of adding a catalyst, namely the glacial acetic acid, the tetraethoxysilane is hydrolyzed into silanol sol, the silanol sol and fiber emulsion are mixed, a heterocomplex containing carbon and silicon is obtained through evaporation solvent, finally high temperature carbonization is conducted, the fiber emulsion provides a carbon source, and a carbon-silicon compound additive is obtained. The carbon-silicon compound additive is stable in chemical property, high in heat conductivity coefficient, low in thermal expansion coefficient, resistant to thermal shock, low in weight and high in strength.

Description

A kind of fluorine silicon resin bonds many carbon refractories and preparation method thereof

Technical field

The present invention relates to a kind of refractory materials, particularly relate to a kind of fluorine silicon resin and to bond many carbon refractories and preparation method thereof.

Background technology

Refractory materials refers to that refractoriness is not less than a class ceramic of 1580 DEG C.Refractoriness refers to that refractory materials cone-shaped body sample is not having in loading situation, resists high temperature action and does not soften molten centigradetemperature.But only define with refractoriness and can not describe refractory materials, 1580 DEG C is not absolute comprehensively.Now be defined as the material that all physicochemical property allow it to use in high temperature environments and be called refractory materials.Refractory materials is widely used in the industrial circles such as metallurgy, chemical industry, oil, machinofacture, silicate, power, and in metallurgical industry, consumption is maximum, accounts for the 50%-60% of ultimate production.

Carbon composite refractory is raw material by two kinds or two or more refractory oxide of different nature and carbon materials and non-oxidic material, the heterogeneous composite refractory of one that carbonaceous organic material is made as bonding agent.The oxide compound adopted mainly contains MgO, Al2O3, ZrO2 and MgAl2O4, carbon is natural graphite mainly, non-oxidized substance is mainly the metals such as Al, Si, Mg, the alloy of AlSi, AlMg class and SiC, B4C mono-compound of class, then in addition shaping by adding the bonding agent such as resin or pitch, the composite refractory be made up of oxide compound, carbon, non-oxygen compound and bonding agent can be obtained.

Summary of the invention

The object of the invention is just to provide a kind of fluorine silicon resin and bonds many carbon refractories and preparation method thereof.

The present invention is achieved by the following technical solutions:

A kind of fluorine silicon resin bonds many carbon refractories, and it is made up of the raw material of following weight parts:

The salpeter solution 3-4 of sisal fibers 10-12, fluorine silicon resin 3-7, tetraethoxy 26-30, crystalline flake graphite 40-53, amorphous graphite 30-40, octadecanoic acid 1-2, tetramethylolmethane 0.7-2, benzotriazole 0.1-0.17,10-13mol/l, Glacial acetic acid 2-3, brown sugar 0.5-1, sodium-potassium silicate 2-3, methylcarbonate 6-8.

Fluorine silicon resin bonds the preparation methods of many carbon refractories, comprises the following steps:

(1) sodium-potassium silicate is joined in 7-10 times of water, be heated to boiling, add brown sugar, be stirred to normal temperature, obtain pre-solution;

(2) sisal fibers being joined concentration is infiltrate 3-4 hour in the bisulfite potassium solution of 5-7%, takes out post-drying, adds salpeter solution, be uniformly mixed 20-30 minute, add edible alkali, regulate PH to be neutral, mix with pre-solution, stir, obtain silica fibre liquid;

(3) tetraethoxy is joined in 8-10 dehydrated alcohol doubly, stirring and dissolving, is added drop-wise in above-mentioned silica fibre liquid, after dropwising by lysate, add Glacial acetic acid, at 40-45 DEG C, react 10-12 hour, with dehydrated alcohol and distilled water, product is washed successively, filter, vacuum calcining: vacuum tightness is 8-10Pa, temperature rise rate is 80-100 DEG C/min, is incubated roasting 10-12 h after being warmed up to 1260-1300 DEG C, obtains carbon silicon composite assistant;

(4) fluorine silicon resin is joined in methylcarbonate, stir, obtain fluorine silicon solution;

(5) by octadecanoic acid, tetramethylolmethane mixing, raised temperature is 76-80 DEG C, insulation reaction 1-2 hour, adds above-mentioned fluorine silicon solution, benzotriazole, is stirred to normal temperature, obtains resin glue;

(6) by crystalline flake graphite, amorphous graphite mixing, mixed rolling 8-10 minute, add resin glue, mixed rolling 6-10 minute, add each raw material of residue, adjustment temperature is 100-110 DEG C, mixed rolling 26-30 minute, hydrostatic profile, forming pressure is 120-130MPa, burns till under buried charcoal atmosphere under 1200-1400 DEG C of condition.

Compared with prior art, advantage of the present invention is:

Tetraethoxy of the present invention is silanol colloidal sol in the Water Under solution that catalyzer Glacial acetic acid adds, silanol colloidal sol is mixed with fibre emulsion, pass through evaporating solvent, obtain the heterocomplex of carbon containing, silicon, eventually pass high temperature cabonization, fibre emulsion provides carbon source, obtains carbon silicon composite assistant, and the stable chemical performance of this carbon silicon composite assistant, thermal conductivity is high, thermal expansivity is little, resistance to thermal shock, lightweight, intensity is high.

Refractory materials of the present invention adopts fluorine silicon resin to be binding agent, has excellent oxidation-resistance, resistance to fouling and hot strength.

Embodiment

Below in conjunction with embodiment, the present invention is described in further detail:

Embodiment 1:

A kind of fluorine silicon resin bonds many carbon refractories, and it is made up of the raw material of following weight parts:

The salpeter solution 4 of sisal fibers 12, fluorine silicon resin 3, tetraethoxy 30, crystalline flake graphite 53, amorphous graphite 30, octadecanoic acid 1, tetramethylolmethane 0.7, benzotriazole 0.17,13mol/l, Glacial acetic acid 3, brown sugar 0.5, sodium-potassium silicate 3, methylcarbonate 6.

Fluorine silicon resin bonds the preparation methods of many carbon refractories, comprises the following steps:

(1) sodium-potassium silicate is joined in 7-10 times of water, be heated to boiling, add brown sugar, be stirred to normal temperature, obtain pre-solution;

(2) sisal fibers being joined concentration is infiltrate 3-4 hour in the bisulfite potassium solution of 5-7%, takes out post-drying, adds salpeter solution, be uniformly mixed 20-30 minute, add edible alkali, regulate PH to be neutral, mix with pre-solution, stir, obtain silica fibre liquid;

(3) tetraethoxy is joined in 8-10 dehydrated alcohol doubly, stirring and dissolving, is added drop-wise in above-mentioned silica fibre liquid, after dropwising by lysate, add Glacial acetic acid, react 12 hours at 45 DEG C, with dehydrated alcohol and distilled water, product is washed successively, filter, vacuum calcining: vacuum tightness is 10Pa, temperature rise rate is 100 DEG C/min, is incubated roasting 12 h after being warmed up to 1300 DEG C, obtains carbon silicon composite assistant;

(4) fluorine silicon resin is joined in methylcarbonate, stir, obtain fluorine silicon solution;

(5) by octadecanoic acid, tetramethylolmethane mixing, raised temperature is 80 DEG C, insulation reaction 2 hours, adds above-mentioned fluorine silicon solution, benzotriazole, is stirred to normal temperature, obtains resin glue;

(6) by crystalline flake graphite, amorphous graphite mixing, mixed rolling 10 minutes, adds resin glue, mixed rolling 10 minutes, add each raw material of residue, adjustment temperature is 110 DEG C, mixed rolling 30 minutes, hydrostatic profile, forming pressure is 130MPa, burns till under buried charcoal atmosphere under 1400 DEG C of conditions.

Performance test:

Refractory materials of the present invention is pressed GB/T13244 and detect oxidation-resistance (1000 DEG C × 3h), practical decarburized depth is 4.5mm; Detecting the heat-shock resistance of 1100 DEG C of water-cooleds by YB/T376.1, there is not crackle in the test that sample can stand 8 times; High temperature break resistant intensity is 7.8MPa.

Claims (2)

1. fluorine silicon resin bonds many carbon refractories, it is characterized in that what it was made up of the raw material of following weight parts:

The salpeter solution 3-4 of sisal fibers 10-12, fluorine silicon resin 3-7, tetraethoxy 26-30, crystalline flake graphite 40-53, amorphous graphite 30-40, octadecanoic acid 1-2, tetramethylolmethane 0.7-2, benzotriazole 0.1-0.17,10-13mol/l, Glacial acetic acid 2-3, brown sugar 0.5-1, sodium-potassium silicate 2-3, methylcarbonate 6-8.

2. fluorine silicon resin as claimed in claim 1 bonds a preparation method for many carbon refractories, it is characterized in that comprising the following steps:

(1) sodium-potassium silicate is joined in 7-10 times of water, be heated to boiling, add brown sugar, be stirred to normal temperature, obtain pre-solution;

(2) sisal fibers being joined concentration is infiltrate 3-4 hour in the bisulfite potassium solution of 5-7%, takes out post-drying, adds salpeter solution, be uniformly mixed 20-30 minute, add edible alkali, regulate PH to be neutral, mix with pre-solution, stir, obtain silica fibre liquid;

(3) tetraethoxy is joined in 8-10 dehydrated alcohol doubly, stirring and dissolving, is added drop-wise in above-mentioned silica fibre liquid, after dropwising by lysate, add Glacial acetic acid, at 40-45 DEG C, react 10-12 hour, with dehydrated alcohol and distilled water, product is washed successively, filter, vacuum calcining: vacuum tightness is 8-10Pa, temperature rise rate is 80-100 DEG C/min, is incubated roasting 10-12 h after being warmed up to 1260-1300 DEG C, obtains carbon silicon composite assistant;

(4) fluorine silicon resin is joined in methylcarbonate, stir, obtain fluorine silicon solution;

(5) by octadecanoic acid, tetramethylolmethane mixing, raised temperature is 76-80 DEG C, insulation reaction 1-2 hour, adds above-mentioned fluorine silicon solution, benzotriazole, is stirred to normal temperature, obtains resin glue;

(6) by crystalline flake graphite, amorphous graphite mixing, mixed rolling 8-10 minute, add resin glue, mixed rolling 6-10 minute, add each raw material of residue, adjustment temperature is 100-110 DEG C, mixed rolling 26-30 minute, hydrostatic profile, forming pressure is 120-130MPa, burns till under buried charcoal atmosphere under 1200-1400 DEG C of condition.