CN116573945A - Corrosion-resistant light-weight fireproof spray paint and preparation method thereof - Google Patents

Corrosion-resistant light-weight fireproof spray paint and preparation method thereof Download PDF

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CN116573945A
CN116573945A CN202310622532.8A CN202310622532A CN116573945A CN 116573945 A CN116573945 A CN 116573945A CN 202310622532 A CN202310622532 A CN 202310622532A CN 116573945 A CN116573945 A CN 116573945A
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stirring
corrosion
spray coating
resistant
calcium
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陈金凤
程水明
张忠
蔡玮
夏昌勇
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China First Metallurgical Group Co Ltd
Wuhan Research Institute of Metallurgical Construction Co Ltd
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China First Metallurgical Group Co Ltd
Wuhan Research Institute of Metallurgical Construction Co Ltd
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Abstract

The invention belongs to the technical field of refractory materials, and discloses an erosion-resistant lightweight refractory spray coating and a preparation method thereof. The preparation method comprises the following steps: step 1, mixing and stirring calcium hexaluminate particles, magnesium aluminate spinel fine powder, alumina fibers, calcium lignosulfonate and calcium aluminate cement to obtain a premix; step 2, adding borax into the premix and stirring to obtain a mixture; step 3, adding water into the mixture and stirring to obtain a precursor material; and step 4, adding sodium oxalate into the precursor material, stirring, and then adding water, stirring to obtain the corrosion-resistant light-weight refractory spray coating. The preparation process is simple, and the prepared spray paint is easy to construct, quick to sinter, high in early strength, good in bonding performance, low in heat conductivity and corrosion resistant, and is widely applicable to lining materials of high-temperature industrial kilns in alkaline working environments.

Description

Corrosion-resistant light-weight fireproof spray paint and preparation method thereof
Technical Field
The invention belongs to the technical field of refractory materials, and particularly relates to an erosion-resistant lightweight refractory spray coating and a preparation method thereof.
Background
The fireproof spray paint is an important component of unshaped fireproof materials, can be divided into dry spray paint and wet spray paint according to different bonding systems, and is widely applied to construction, repair and the like of high-temperature industrial kiln linings. Unlike shaped products or prefabricated parts, the fireproof spray paint has no preforming process, is mainly adhered by means of a bonding system of the material, and can generate sintering strength under the high temperature condition of kiln service, so that the fireproof spray paint needs to meet the following requirements:
(1) The rebound rate is low. The spray paint is adhered to the lining of the high-temperature kiln through the spraying equipment, but part of the spray paint still can rebound and fall off, and the reduction of the rebound rate of the fire-resistant spray paint is always the focus of research work.
(2) The sintering performance is good. The spray coating, whether used as a lining or repair material, needs to be able to sinter quickly and form good sinter fusion and integrity with the substrate.
(3) The bonding performance is strong. The selection of the fire-resistant spray paint binder needs to be determined according to the main material, and good binding performance is an important guarantee of early strength of the spray paint.
(4) The anti-stripping performance is excellent. In the service process of the high-temperature kiln, the spray coating is easy to generate pore or crack initiation structure peeling due to the escape of the bonding agent.
(5) Has good heat insulation effect and corrosion resistance. The spray coating is preferably made of a main material with light material and small specific gravity, not only has good heat insulation effect, but also can reduce the dead weight of the material and prevent early rebound from falling off, and the heat insulation and corrosion resistance are in certain opposition, and the spray coating maintains certain porosity, so that the heat insulation and the corrosion resistance are damaged.
Patent CN115124367a discloses an acid and alkali corrosion resistant spray coating for cement kiln and a preparation method thereof, by adding ultrafine powder and pore-forming agent, the spray coating has the advantages of high density and relatively high aperture ratio, the acid and alkali corrosion resistant performance is ensured, the weight is not too large, the normal use of the cement kiln is not affected, but the stripping resistance of the spray coating is remarkably and negatively affected by the aperture. Patent CN101492305a discloses a mullite refractory spray coating, which takes mullite, pure calcium aluminate cement, silica fume and the like as raw materials, and forms communicated pores by adding an explosion-proof agent, so that the purpose of quick-drying and explosion prevention is achieved, but the formation of the communicated pores can greatly reduce the erosion resistance of the spray coating. It can be seen that meeting the above requirements at the same time has great difficulty.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides the corrosion-resistant light-weight refractory spray paint and the preparation method thereof, the preparation process is simple, the prepared spray paint is easy to construct, quick to sinter, high in early strength, good in bonding performance, and has the characteristics of low heat conductivity and corrosion resistance, and the spray paint is widely applicable to lining materials of high-temperature industrial kilns in alkaline working environments.
In order to solve the technical problem, the invention provides a preparation method of an erosion-resistant lightweight refractory spray coating, which comprises the following steps:
step 1, mixing and stirring calcium hexaluminate particles, magnesium aluminate spinel fine powder, alumina fibers, calcium lignosulfonate and calcium aluminate cement to obtain a premix;
step 2, adding borax into the premix and stirring to obtain a mixture;
step 3, adding water into the mixture and stirring to obtain a precursor material;
and step 4, adding sodium oxalate into the precursor material, stirring, and then adding water, stirring to obtain the corrosion-resistant light-weight refractory spray coating.
In the scheme, the mass ratio of the calcium hexaluminate particles, the magnesium aluminate spinel fine powder, the alumina fibers, the calcium lignosulfonate and the calcium aluminate cement is 100:25-30:12-18:0.5-1.5:6-10.
In the scheme, the addition amount of the borax is 2.5-4.5% of the mass of the premix.
In the scheme, the addition amount of the sodium oxalate is 0.5-1.5% of the mass of the precursor.
In the scheme, the adding amount of water in the step 3 is 2-3% of the mass of the mixture; the addition amount of water in the step 4 is 2-4% of the mass of the precursor.
In the scheme, the stirring speed in the steps 1 to 4 is 40-50 r/min.
In the scheme, the stirring time of the step 1 is 15-20 min, the stirring time of the step 2 is 5-6 min, and the stirring time of the step 3 is 3-5 min; in the step 4, the stirring time after adding sodium oxalate is 3-5 min, and the stirring time after adding water is 2-3 min.
In the scheme, the granularity of the calcium hexaluminate particles is graded as that the mass ratio of the particles with the particle diameter of 0.1-0.3 mm, the particle diameter of 0.8-1 mm and the particle diameter of 1.3-1.5 mm is 100:15-30:10-15; the CaO content of the calcium hexaluminate particles is 8-10%, and the sphericity is 0.8-0.85.
In the scheme, the granularity of the magnesia-alumina spinel fine powder is 70-80 mu m, al 2 O 3 The content is 70-75%.
In the above scheme, the alumina fiber is Al 2 O 3 The content is 80-90%, the length is 1-4 mm, and the diameter is 15-20 μm.
In the scheme, the calcium lignosulfonate, the calcium aluminate cement, the borax and the sodium oxalate are all industrially pure.
The invention also provides an erosion-resistant lightweight refractory spray coating, which is prepared by the method.
In the scheme, the rebound rate of the corrosion-resistant light-weight refractory spray coating is 2-3%, and the volume density of the spray coating after being dried at 110 ℃ for 12 hours is 2.38-2.65 g/cm 3 The normal temperature compressive strength after being dried at 110 ℃ for 12 hours is 40-45 MPa, the heat conductivity coefficient after being burned at 1400 ℃ for 3 hours is 1.6-1.8W/(m.K), the high temperature flexural strength at 1400 ℃ for 1 hour is 8.5-12.8 MPa, and the erosion index of a static crucible method slag resistance test at 1100 ℃ for 3 hours is 1.8-2.5%.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the invention, through a step-by-step adding means, namely, barren materials are fully premixed, then bonding agents and the like are added, and a rapid stirring process is combined, so that on one hand, the hardening of raw material components is regulated, the full contact of raw materials of all components is enhanced, on the other hand, the bleeding property of the spray coating is reduced, and the plasticity and the bonding force of the spray coating are improved.
(2) According to the invention, spherical calcium hexaluminate particles are used as aggregate, and aggregate space architecture is formed through grading intermittent distribution, so that the weight of the spray coating is reduced, the heat conductivity coefficient of the calcium hexaluminate is low, the magnesium aluminate spinel and the calcium hexaluminate have good chemical erosion resistance, and the erosion resistance of the spray coating is effectively improved.
(3) The invention uses the hydration of calcium aluminate cement to generate good early strength, uses the alumina fiber as bridging, is inlaid in the chip structure of the hydration product of the calcium aluminate cement to play a role of connection, is beneficial to the discharge of gases such as moisture, reduces the rebound rate of the spray coating and improves the workability of the spray coating.
(4) The invention utilizes borax to hydrolyze and form B (OH) 4– The long chain of the group generates chemical combination, so that the combination property of the spray paint is improved; and a liquid phase is generated under the high-temperature service condition, and the rapid sintering and fusion of the material are promoted through the in-situ formation of ceramic phases such as aluminum borate and the like, so that the high-temperature spalling resistance of the spray coating is effectively improved.
(5) According to the invention, the hardening rate of cement is regulated by introducing sodium oxalate, so that the construction time of the spray paint is prolonged; in addition, the corrosion reaction of sodium oxalate and alumina fiber at high temperature promotes the connection of calcium hexaluminate spherical material, improves the sintering bonding strength of aggregate-matrix, and further improves the erosion resistance of the spray material.
Therefore, the invention has the characteristics of simple preparation process, and the prepared corrosion-resistant light-weight fireproof spray paint is easy to construct, quick to sinter, high in early strength, good in combination property, low in heat conductivity coefficient and corrosion-resistant, and is widely applicable to lining materials of high-temperature industrial kilns in alkaline working environments.
Detailed Description
For a better understanding of the present invention, the following examples are further illustrated, but are not limited to the following examples.
In the following examples, the CaO content of the calcium hexaluminate particles is 8-10% and the sphericity is 0.8-0.85; the granularity of the adopted magnesia-alumina spinel fine powder is 70-80 mu m, al 2 O 3 The content is 70-75 percent; al of the alumina fibers used 2 O 3 The content is 80-90%, the length is 1-4 mm, and the diameter is 15-20 μm; the adopted calcium lignosulfonate, calcium aluminate cement, borax and sodium oxalate are all industrially pure.
In the following examples, the rebound resilience was measured by the method of GB/T41503-2022, the bulk density was measured by the method of YB/T5200-1993, the compressive strength was measured by the method of GB/T5072-2008, the heat conductivity was measured by the method of GB/T4130-2005, the high temperature flexural strength was measured by the method of GB/T3002-2017, and the erosion area percentage was measured as an erosion index by the static crucible slag resistance test using the method of GB/T8931-2007.
Example 1
A preparation method of corrosion-resistant lightweight refractory spray paint comprises the following steps:
step 1, mixing calcium hexaluminate particles, magnesium aluminate spinel fine powder, alumina fibers, calcium lignosulfonate and calcium aluminate cement according to a mass ratio of 100:27:15:0.8:6, and stirring for 15min to obtain a premix;
step 2, adding borax accounting for 2.8% of the mass of the premix into the premix, and stirring for 5min to obtain a mixture;
step 3, adding water accounting for 2% of the mass of the mixture into the mixture, and stirring for 5min to obtain a precursor;
and 4, adding sodium oxalate accounting for 0.8% of the mass of the precursor into the precursor, stirring for 3min, adding water accounting for 3% of the mass of the precursor, and stirring for 2min to obtain the corrosion-resistant light-weight refractory spray coating.
In the preparation step, the granularity of the adopted calcium hexaluminate particles is graded as that the mass ratio of the particles with the particle diameter of 0.1-0.3 mm, the particle diameter of 0.8-1 mm and the particle diameter of 1.3-1.5 mm is 100:25:12; the stirring rate in each of the steps 1 to 4 was 45r/min.
This practice isThe corrosion-resistant light-weight refractory spray paint prepared in the example is detected: the rebound rate is 2%; the volume density after drying at 110 ℃ for 12h is 2.47g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The normal temperature compressive strength is 43MPa after being dried at 110 ℃ for 12 hours; the heat conductivity coefficient after being burned at 1400 ℃ for 3 hours is 1.6W/(m.K); 1400 ℃ x 1h high temperature flexural strength 9.7MPa; the erosion index of the slag resistance test of the 1100 ℃ x 3h static crucible method is 2.2%.
Example 2
A preparation method of corrosion-resistant lightweight refractory spray paint comprises the following steps:
step 1, mixing calcium hexaluminate particles, magnesium aluminate spinel fine powder, alumina fibers, calcium lignosulfonate and calcium aluminate cement according to a mass ratio of 100:30:12:1.2:8, and stirring for 16min to obtain a premix;
step 2, adding borax accounting for 3.2% of the mass of the premix into the premix, and stirring for 6min to obtain a mixture;
step 3, adding water accounting for 2.5% of the mass of the mixture into the mixture, and stirring for 3min to obtain a precursor;
and 4, adding sodium oxalate accounting for 1.2% of the mass of the precursor into the precursor, stirring for 4min, adding water accounting for 4% of the mass of the precursor, and stirring for 3min to obtain the corrosion-resistant light-weight refractory spray coating.
In the preparation step, the granularity of the adopted calcium hexaluminate particles is graded as that the mass ratio of the particles with the particle diameter of 0.1-0.3 mm, the particle diameter of 0.8-1 mm and the particle diameter of 1.3-1.5 mm is 100:18:15; the stirring rate in each of the steps 1 to 4 was 48r/min.
The corrosion-resistant light-weight refractory spray paint prepared in the embodiment is detected by the following steps: the rebound rate is 3%; the volume density after drying at 110 ℃ for 12h is 2.55g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The normal temperature compressive strength is 42MPa after being dried at 110 ℃ for 12 hours; the heat conductivity coefficient after being burned at 1400 ℃ for 3 hours is 1.8W/(m.K); 1400 ℃ x 1h high temperature flexural strength 11.5MPa; the erosion index of the slag resistance test of the 1100 ℃ x 3h static crucible method is 1.8%.
Example 3
A preparation method of corrosion-resistant lightweight refractory spray paint comprises the following steps:
step 1, mixing calcium hexaluminate particles, magnesium aluminate spinel fine powder, alumina fibers, calcium lignosulfonate and calcium aluminate cement according to a mass ratio of 100:26:16:0.6:9, and stirring for 18min to obtain a premix;
step 2, adding borax accounting for 4% of the mass of the premix into the premix, and stirring for 5min to obtain a mixture;
step 3, adding water accounting for 3% of the mass of the mixture into the mixture, and stirring for 4min to obtain a precursor;
and 4, adding sodium oxalate accounting for 0.6% of the mass of the precursor into the precursor, stirring for 3min, adding water accounting for 3% of the mass of the precursor, and stirring for 2min to obtain the corrosion-resistant light-weight refractory spray coating.
In the preparation step, the granularity of the adopted calcium hexaluminate particles is graded as that the mass ratio of the particles with the particle diameter of 0.1-0.3 mm, the particle diameter of 0.8-1 mm and the particle diameter of 1.3-1.5 mm is 100:20:10; the stirring rate in each of the steps 1 to 4 was 50r/min.
The corrosion-resistant light-weight refractory spray paint prepared in the embodiment is detected by the following steps: the rebound rate is 3%; the volume density after drying at 110 ℃ for 12h is 2.52g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The normal temperature compressive strength is 40MPa after being dried at 110 ℃ for 12 hours; the heat conductivity coefficient after being burned at 1400 ℃ for 3 hours is 1.6W/(m.K); 1400 ℃ x 1h high temperature flexural strength 8.5MPa; the erosion index of the slag resistance test of the 1100 ℃ x 3h static crucible method is 2.3%.
Comparative example 1
A preparation method of the spray paint comprises the following steps:
step 1, mixing calcium hexaluminate particles, magnesium aluminate spinel fine powder, alumina fibers, calcium lignosulfonate and calcium aluminate cement according to a mass ratio of 100:40:10:2:4, and stirring for 15min to obtain a premix;
step 2, adding borax accounting for 2% of the mass of the premix into the premix, and stirring for 5min to obtain a mixture;
step 3, adding water accounting for 1% of the mass of the mixture into the mixture, and stirring for 5min to obtain a precursor;
and 4, adding sodium oxalate accounting for 2% of the mass of the precursor into the precursor, stirring for 3min, adding water accounting for 5% of the mass of the precursor, and stirring for 5min to obtain the spray coating.
In the preparation step, the granularity of the adopted calcium hexaluminate particles is graded as that the mass ratio of the particles with the particle diameter of 0.1-0.5 mm, the particle diameter of 0.5-1 mm (without 0.5 mm) and the particle diameter of 1-1.5 mm (without 1 mm) is 100:30:30; the stirring rate in each of the steps 1 to 4 was 25r/min.
The spray paint prepared in this comparative example was tested: the rebound rate is 5%; the volume density after drying at 110 ℃ for 12h is 2.24g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The normal temperature compressive strength is 35MPa after being dried at 110 ℃ for 12 hours; the heat conductivity coefficient after being burned at 1400 ℃ for 3 hours is 1.5W/(m.K); 1400 ℃ x 1h high temperature flexural strength 6.6MPa; the erosion index of the slag resistance test of the 1100 ℃ x 3h static crucible method is 4.7%.
From the test data of example 1 and comparative example 1, it can be seen that: the raw material components have obvious influence on the performance of the spray paint. Under the condition of similar preparation process, the adjustment of the content of raw material components, the change of the granularity grading of raw materials and the reduction of stirring rate cause the reduction of the bonding and sintering performance of the spray coating, the damage of the high-temperature mechanical property (the reduction of high-temperature flexural strength) of the spray coating and the weakening of the slag resistance (the increase of erosion index) of the spray coating.
Comparative example 2
A preparation method of the spray paint comprises the following steps:
step 1, mixing calcium hexaluminate particles, magnesium aluminate spinel fine powder, alumina fibers, calcium lignosulfonate and calcium aluminate cement according to a mass ratio of 100:27:15:0.8:6, and stirring for 15min to obtain a premix;
and 2, adding borax accounting for 2.8% of the mass of the premix, sodium oxalate accounting for 0.8% of the mass of the premix and water accounting for 5% of the mass of the premix into the premix, and stirring for 15min to obtain the spray coating.
In the preparation step, the granularity of the adopted calcium hexaluminate particles is graded as that the mass ratio of the particles with the particle diameter of 0.1-0.3 mm, the particle diameter of 0.8-1 mm and the particle diameter of 1.3-1.5 mm is 100:25:12; the stirring rate in each of the steps 1 to 2 was 40r/min.
The spray paint prepared in this comparative example was tested: the rebound rate is 6%; the volume density after drying at 110 ℃ for 12h is 2.22g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the Normal temperature compressive strength after drying at 110 ℃ for 12h25MPa; the heat conductivity coefficient after being burned at 1400 ℃ for 3 hours is 2.1W/(m.K); 1400 ℃ x 1h high temperature flexural strength 5.8MPa; the erosion index of the slag resistance test of the 1100 ℃ x 3h static crucible method is 6.4%.
From the test data of example 1 and comparative example 2, it can be seen that: the preparation process is an important influencing factor of the performance of the spray coating. Under the condition that the raw material components are similar, the normal temperature and high temperature mechanical properties of the prepared spray coating are reduced by means of one-time feeding and integral mixing, and the slag resistance performance is deteriorated.
The above examples are presented for clarity of illustration only and are not limiting of the embodiments. Other variations or modifications of the above description will be apparent to those of ordinary skill in the art, and it is not necessary or exhaustive of all embodiments, and thus all obvious variations or modifications that come within the scope of the invention are desired to be protected.

Claims (10)

1. The preparation method of the corrosion-resistant light-weight refractory spray paint is characterized by comprising the following steps of:
step 1, mixing and stirring calcium hexaluminate particles, magnesium aluminate spinel fine powder, alumina fibers, calcium lignosulfonate and calcium aluminate cement to obtain a premix;
step 2, adding borax into the premix and stirring to obtain a mixture;
step 3, adding water into the mixture and stirring to obtain a precursor material;
and step 4, adding sodium oxalate into the precursor material, stirring, and then adding water, stirring to obtain the corrosion-resistant light-weight refractory spray coating.
2. The method for preparing the corrosion-resistant lightweight refractory spray coating according to claim 1, wherein the mass ratio of the calcium hexaluminate particles, the magnesium aluminate spinel fine powder, the alumina fibers, the calcium lignosulfonate and the calcium aluminate cement is 100:25-30:12-18:0.5-1.5:6-10.
3. The method for preparing the corrosion-resistant light-weight refractory spray paint according to claim 1, wherein the addition amount of borax is 2.5-4.5% of the mass of the premix; the addition amount of the sodium oxalate is 0.5-1.5% of the mass of the precursor.
4. The method for preparing the corrosion-resistant light-weight refractory spray paint according to claim 1, wherein the water added in the step 3 is 2-3% of the mass of the mixture; the addition amount of water in the step 4 is 2-4% of the mass of the precursor.
5. The method for preparing the corrosion-resistant light-weight refractory spray coating according to claim 1, wherein the stirring rate in the steps 1 to 4 is 40-50 r/min; the stirring time of the step 1 is 15-20 min, the stirring time of the step 2 is 5-6 min, and the stirring time of the step 3 is 3-5 min; in the step 4, the stirring time after adding sodium oxalate is 3-5 min, and the stirring time after adding water is 2-3 min.
6. The method for preparing the corrosion-resistant light-weight refractory spray paint according to claim 1, wherein the calcium hexaluminate particles are prepared by the particle size grading of 100:15-30:10-15, wherein the particle mass ratio of 0.1-0.3 mm in particle size, 0.8-1 mm in particle size and 1.3-1.5 mm in particle size; the CaO content of the calcium hexaluminate particles is 8-10%, and the sphericity is 0.8-0.85.
7. The method for preparing the corrosion-resistant light-weight refractory spray coating according to claim 1, wherein the particle size of the magnesia-alumina spinel fine powder is 70-80 μm, and Al 2 O 3 The content is 70-75%.
8. The method of preparing an erosion resistant lightweight refractory spray coating according to claim 1, wherein the oxidizingAl of aluminum fibers 2 O 3 The content is 80-90%, the length is 1-4 mm, and the diameter is 15-20 μm.
9. An erosion-resistant lightweight refractory spray coating prepared by the method of any one of claims 1-8.
10. The corrosion-resistant lightweight refractory spray coating according to claim 9, wherein the corrosion-resistant lightweight refractory spray coating has a rebound rate of 2 to 3% and a bulk density of 2.38 to 2.65g/cm after drying at 110 ℃ x 12h 3 The normal temperature compressive strength after being dried at 110 ℃ for 12 hours is 40-45 MPa, the heat conductivity coefficient after being burned at 1400 ℃ for 3 hours is 1.6-1.8W/(m.K), the high temperature flexural strength at 1400 ℃ for 1 hour is 8.5-12.8 MPa, and the erosion index of a static crucible method slag resistance test at 1100 ℃ for 3 hours is 1.8-2.5%.
CN202310622532.8A 2023-05-30 2023-05-30 Corrosion-resistant light-weight fireproof spray paint and preparation method thereof Pending CN116573945A (en)

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