A welding fireproof cotton and its preparation method

Abstract

This invention discloses a welding fireproof cotton and its preparation method, belonging to the field of fireproof material preparation. This invention uses magnesium hydroxide and phosphorus-doped biochar in combination, which not only interacts with other base materials to form a good flame-retardant system, but also synergistically enhances the effect with antioxidants, achieving a more significant fireproofing purpose. Furthermore, the synergistic effect of modified perlite powder and composite fibers increases the system's high-temperature resistance. Specifically, the introduction of phosphorus, a highly effective flame-retardant element, into the biochar, followed by high-temperature pyrolysis, allows phytic acid to form a phosphorus-containing carbonized layer that is difficult to burn, optimizing the material's molecular structure and further improving the system's fireproof performance. Additionally, the modified perlite powder also incorporates phosphorus, synergistically enhancing flame retardancy. Moreover, the silane coupling agent increases its compatibility within the system, contributing to a fireproof layer with superior uniformity, adhesion, and flame retardancy.

Description

Technical Field

[0001] This invention relates to the field of fireproof material preparation, and more specifically, to a welding fireproof cotton and its preparation method. Background Technology

[0002] In electric welding operations, fire-fighting devices are rarely used to collect sparks, which leads to certain safety hazards. This not only affects the health of welders but can also cause fires in severe cases. Therefore, developing a safe and effective fireproof cotton for welding is of great significance.

[0003] Existing technologies also include related fire-resistant products, such as welding blankets and fire blankets. These products are mainly made of fire-retardant and non-combustible fibers, processed through special techniques. Their main characteristics are non-combustibility, high temperature resistance (550–1100℃), dense structure, non-irritating properties, and soft yet resilient texture, making them convenient for wrapping objects and equipment with uneven surfaces. Welding blankets, in particular, effectively protect objects from heat sources and spark zones, completely preventing or isolating combustion. During welding, welding blankets are laid on both sides of the object to prevent sparks from contacting the object or from splashing out. This application uses alumina fiber as the matrix layer. Alumina fiber has a long-term service temperature of 1400℃ and a maximum service temperature of 1600℃. Compared to other materials, it has higher fire resistance and a significant advantage in fire protection under high-temperature flames. However, a single alumina fiber layer has weak resistance to flame impact, poor fire resistance, and a short fire resistance time, limiting its application. Furthermore, there is still room for improvement in its high-temperature flame-retardant performance. Summary of the Invention

[0004] Therefore, in order to address the problems of poor fire resistance and the urgent need to improve flame retardant properties in existing fireproof cotton, this invention provides a weldable fireproof cotton and its preparation method, the specific technical solution of which is as follows:

[0005] A welding fireproof cotton, comprising a base layer and a fireproof layer wrapped around the surface of the base layer, wherein the fireproof layer comprises the following raw materials by weight:

[0006] The composition includes 35-38 parts polyester resin, 9-11 parts nano silica, 3-5 parts hydroxypropyl cellulose, 1-7 parts composite fiber, 3-9 parts flame retardant, 3-9 parts modified perlite powder, 1-5 parts antioxidant, 1-2 parts dispersant, 1-2 parts defoamer, 1-3 parts leveling agent, and 10-15 parts water.

[0007] The flame retardant is obtained by mixing magnesium hydroxide and phosphorus-doped biochar in a mass ratio of (1-3):(1-2).

[0008] Furthermore, the polyester resin is a carboxyl polyester resin with an acid value between 60 mg KOH / g and 80 mg KOH / g.

[0009] Furthermore, the composite fiber is obtained by mixing ceramic fiber, glass fiber and aluminosilicate fiber in a mass ratio of (1-5):(1-3):(1-9).

[0010] Further, the preparation method of the modified perlite powder is as follows: the perlite powder is heat-treated at 250℃~350℃ for 15min~30min, then cooled to 60℃~65℃, a phosphoric acid solution with pH 5.5 is added, and the mixture is stirred for 20min~30min. Then a silane coupling agent solution is added, and the mixture is stirred for another 15min~30min. After washing with water and drying, the modified perlite powder is obtained.

[0011] Furthermore, the phosphoric acid solution has a mass percentage concentration of 5% to 15%, and the silane coupling agent solution has a mass percentage concentration of 3% to 10%.

[0012] Furthermore, the preparation method of the phosphorus-doped biochar is as follows: place the biochar in a phytic acid solution, mix evenly, then heat treat at 250℃~300℃ for 3h~5h, cool to room temperature, and dry to obtain phosphorus-doped biochar.

[0013] Furthermore, the phytic acid solution has a mass percentage concentration of 10% to 15%.

[0014] Furthermore, the substrate layer is an alumina-based fiber layer.

[0015] Furthermore, the antioxidant is at least one of N-benzylamine phenylenediamine and N,N-diphenyl-p-phenylenediamine.

[0016] In addition, the present invention also provides a method for preparing welding fireproof cotton, the method comprising the following steps:

[0017] Polyester resin, nano silica, hydroxypropyl cellulose, composite fiber, dispersant, defoamer, leveling agent and water are added to a reaction vessel, heated to 65℃~85℃, and treated with a stirring speed of 200r / min~300r / min for 30min~40min. Then flame retardant, modified perlite powder and antioxidant are added, and treated with a stirring speed of 350r / min~500r / min for 50min~60min to obtain slurry.

[0018] The slurry is coated onto the surface of the substrate layer and dried to obtain welding fireproof cotton.

[0019] Compared with the prior art, the present invention has the following beneficial effects:

[0020] 1. This invention uses magnesium hydroxide and phosphorus-doped biochar in combination, which not only interacts with other base materials to form a good flame retardant system, but also synergistically enhances the effect with antioxidants to achieve a more significant fire prevention purpose. Furthermore, with the synergistic effect of modified perlite powder, the high temperature resistance of the system can be increased.

[0021] 2. This invention optimizes the material's molecular structure by introducing phosphorus, which has a significant flame-retardant effect, into biochar. Through high-temperature pyrolysis, phytic acid and biochar form a phosphorus-containing carbonized layer that is difficult to burn. This further improves the fire resistance of the system. In addition, phosphorus is also introduced into the modified perlite powder, which synergistically retards the flame. Furthermore, under the action of a silane coupling agent, its compatibility in the system is increased, which helps to improve its dispersibility and obtain a fireproof layer with better uniformity, adhesion, and flame retardancy.

[0022] 3. This invention optimizes the raw materials for preparing the fireproof layer, ensuring its excellent flame-retardant and fire-resistant performance. By adding composite fibers, it helps to improve both the fire-resistant performance and the strength of the fireproof layer. The overall preparation process is controllable and highly operable. Detailed Implementation

[0023] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to its embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the scope of protection of the invention.

[0024] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and / or" as used herein includes any and all combinations of one or more of the associated listed items.

[0025] A welding fireproof cotton according to one embodiment of the present invention includes a base layer and a fireproof layer wrapped around the surface of the base layer, wherein the fireproof layer comprises the following raw materials by weight:

[0026] The composition includes 35-38 parts polyester resin, 9-11 parts nano silica, 3-5 parts hydroxypropyl cellulose, 1-7 parts composite fiber, 3-9 parts flame retardant, 3-9 parts modified perlite powder, 1-5 parts antioxidant, 1-2 parts dispersant, 1-2 parts defoamer, 1-3 parts leveling agent, and 10-15 parts water.

[0027] The flame retardant is obtained by mixing magnesium hydroxide and phosphorus-doped biochar in a mass ratio of (1-3):(1-2).

[0028] In one embodiment, the polyester resin is a carboxyl polyester resin with an acid value between 60 mg KOH / g and 80 mg KOH / g.

[0029] In one embodiment, the composite fiber is obtained by mixing ceramic fiber, glass fiber and aluminosilicate fiber in a mass ratio of (1-5):(1-3):(1-9).

[0030] In one embodiment, the diameter of a single fiber of the composite fiber is 2μm to 5μm.

[0031] In one embodiment, the modified perlite powder is prepared by: heat-treating the perlite powder at 250℃~350℃ for 15min~30min, then cooling it to 60℃~65℃, adding a phosphoric acid solution with pH 5.5, stirring for 20min~30min, then adding a silane coupling agent solution, continuing to stir for 15min~30min, washing with water, and drying to obtain the modified perlite powder.

[0032] In one embodiment, the phosphoric acid solution has a mass percentage concentration of 5% to 15%, and the silane coupling agent solution has a mass percentage concentration of 3% to 10%.

[0033] In one embodiment, the preparation method of the phosphorus-doped biochar is as follows: biochar is placed in phytic acid solution, mixed evenly, and then heat-treated at 250℃~300℃ for 3h~5h. After cooling to room temperature, it is dried to obtain phosphorus-doped biochar.

[0034] In one embodiment, the phytic acid solution has a mass percentage concentration of 10% to 15%.

[0035] In one embodiment, the biochar is porous biochar with a specific surface area of ​​1500 m². 2 / g~2000m 2 / g.

[0036] In one embodiment, the substrate layer is an alumina-based fiber layer.

[0037] In one embodiment, the antioxidant is at least one of N-benzylamine phenylenediamine and N,N-diphenyl-p-phenylenediamine.

[0038] In one embodiment, the dispersant is at least one of polyethylene glycol, polyvinylpyrrolidone, and sodium hexametaphosphate.

[0039] In one embodiment, the defoamer is at least one selected from tributyl phosphate, dodecyl alcohol, hexadecyl alcohol, and octyl alcohol.

[0040] In one embodiment, the leveling agent is a silicone leveling agent.

[0041] In addition, the present invention also provides a method for preparing welding fireproof cotton, the method comprising the following steps:

[0042] Polyester resin, nano silica, hydroxypropyl cellulose, composite fiber, dispersant, defoamer, leveling agent and water are added to a reaction vessel, heated to 65℃~85℃, and treated with a stirring speed of 200r / min~300r / min for 30min~40min. Then flame retardant, modified perlite powder and antioxidant are added, and treated with a stirring speed of 350r / min~500r / min for 50min~60min to obtain slurry.

[0043] The slurry is coated onto the surface of the substrate layer and dried to obtain welding fireproof cotton.

[0044] In one embodiment, the coating thickness of the slurry is 1 mm to 3 mm.

[0045] In one embodiment, the drying process is carried out at a temperature of 120°C to 125°C for a duration of 1 hour to 3 hours.

[0046] The above solution optimizes the raw materials used in the preparation of the fireproof layer, ensuring its strength while achieving a significant flame-retardant and fire-resistant effect.

[0047] The implementation schemes of the present invention will now be described in detail with reference to specific embodiments.

[0048] Example 1:

[0049] A welding fireproof cotton, comprising a base layer and a fireproof layer wrapped around the surface of the base layer, wherein in this embodiment the base layer is an alumina-based fiber layer; and the fireproof layer comprises the following raw materials by weight:

[0050] The composition comprises 36 parts polyester resin, 10 parts nano silica, 4 parts hydroxypropyl cellulose, 6 parts composite fiber, 6 parts flame retardant, 5 parts modified perlite powder, 3 parts N-benzylamine phenylenediamine, 1 part sodium hexametaphosphate, 1 part hexadecyl alcohol, 2 parts organosilicon leveling agent, and 13 parts water; wherein the flame retardant is obtained by mixing magnesium hydroxide and phosphorus-doped biochar in a mass ratio of 2:1; the composite fiber is obtained by mixing ceramic fiber, glass fiber, and aluminosilicate fiber in a mass ratio of 2:1:3, and the single fiber diameter of the composite fiber is 2 μm;

[0051] A method for preparing welding fireproof cotton includes the following steps:

[0052] The perlite powder was heat-treated at 300℃ for 20 min, then cooled to 60℃, and a 10% (w / w) phosphoric acid solution was added. The mixture was stirred for 25 min, and then a 5% (w / w) silane coupling agent solution was added. The mixture was stirred for another 15 min, washed with water, and dried to obtain modified perlite powder.

[0053] With a surface area of ​​1800m 2 / g of biochar was placed in a phytic acid solution with a mass percentage concentration of 12%, mixed evenly, and then heat-treated at 300℃ for 3h. After cooling to room temperature, it was dried to obtain phosphorus-doped biochar.

[0054] Polyester resin, nano silica, hydroxypropyl cellulose, composite fiber, sodium hexametaphosphate, hexadecyl alcohol, silicone leveling agent and water are added to a reaction vessel, heated to 70°C and treated with a stirring speed of 200 r / min for 30 min. Then flame retardant, modified perlite powder and N-benzylamine phenylenediamine are added and treated with a stirring speed of 350 r / min for 60 min to obtain slurry.

[0055] The slurry was coated onto the surface of the alumina-based fiber layer with a coating thickness of 3 mm, and then dried at 120°C for 2 hours to obtain welding fireproof cotton.

[0056] Example 2:

[0057] A welding fireproof cotton, comprising a base layer and a fireproof layer wrapped around the surface of the base layer, wherein in this embodiment the base layer is an alumina-based fiber layer; and the fireproof layer comprises the following raw materials by weight:

[0058] The composition comprises 38 parts polyester resin, 11 parts nano silica, 3 parts hydroxypropyl cellulose, 7 parts composite fiber, 5 parts flame retardant, 7 parts modified perlite powder, 2 parts N-benzylamine phenylenediamine, 1 part sodium hexametaphosphate, 1 part tributyl phosphate, 1 part organosilicon leveling agent, and 12 parts water; wherein the flame retardant is obtained by mixing magnesium hydroxide and phosphorus-doped biochar in a mass ratio of 3:2; the composite fiber is obtained by mixing ceramic fiber, glass fiber, and aluminosilicate fiber in a mass ratio of 2:2:3, and the single fiber diameter of the composite fiber is 2 μm;

[0059] A method for preparing welding fireproof cotton includes the following steps:

[0060] Perlite powder was heat-treated at 320℃ for 25 min, then cooled to 65℃, and a phosphoric acid solution with a mass percentage concentration of 11% was added. The mixture was stirred for 30 min, and then a silane coupling agent solution with a mass percentage concentration of 8% was added. The mixture was stirred for another 15 min, washed with water, and dried to obtain modified perlite powder.

[0061] With a surface area of ​​2000m 2 / g of biochar was placed in a 15% phytic acid solution, mixed evenly, and then heat-treated at 300℃ for 4h. After cooling to room temperature, it was dried to obtain phosphorus-doped biochar.

[0062] Polyester resin, nano silica, hydroxypropyl cellulose, composite fiber, sodium hexametaphosphate, tributyl phosphate, silicone leveling agent and water are added to a reaction vessel, heated to 75°C and treated with a stirring speed of 300 r / min for 35 min. Then flame retardant, modified perlite powder and N-benzylamine phenylenediamine are added and treated with a stirring speed of 400 r / min for 55 min to obtain slurry.

[0063] The slurry was coated onto the surface of the alumina-based fiber layer with a coating thickness of 3 mm, and then dried at 125°C for 2 hours to obtain welding fireproof cotton.

[0064] Example 3:

[0065] A welding fireproof cotton, comprising a base layer and a fireproof layer wrapped around the surface of the base layer, wherein in this embodiment the base layer is an alumina-based fiber layer; and the fireproof layer comprises the following raw materials by weight:

[0066] The composition comprises 37 parts polyester resin, 10 parts nano silica, 4 parts hydroxypropyl cellulose, 5 parts composite fiber, 8 parts flame retardant, 4 parts modified perlite powder, 1 part N-benzylamine phenylenediamine, 1 part sodium hexametaphosphate, 1 part tributyl phosphate, 1 part organosilicon leveling agent, and 11 parts water; wherein the flame retardant is obtained by mixing magnesium hydroxide and phosphorus-doped biochar in a mass ratio of 3:1; the composite fiber is obtained by mixing ceramic fiber, glass fiber, and aluminosilicate fiber in a mass ratio of 1:1:3, and the single fiber diameter of the composite fiber is 2 μm;

[0067] A method for preparing welding fireproof cotton includes the following steps:

[0068] Perlite powder was heat-treated at 350℃ for 20 min, then cooled to 65℃, and a 12% (w / w) phosphoric acid solution was added. The mixture was stirred for 25 min, and then a 10% (w / w) silane coupling agent solution was added. The mixture was stirred for another 20 min, washed with water, and dried to obtain modified perlite powder.

[0069] With a surface area of ​​1900m 2 / g of biochar was placed in a phytic acid solution with a mass percentage concentration of 12%, mixed evenly, and then heat-treated at 280℃ for 5h. After cooling to room temperature, it was dried to obtain phosphorus-doped biochar.

[0070] Polyester resin, nano silica, hydroxypropyl cellulose, composite fiber, sodium hexametaphosphate, tributyl phosphate, silicone leveling agent and water are added to a reaction vessel, heated to 75°C and treated with a stirring speed of 300 r / min for 40 min. Then flame retardant, modified perlite powder and N-benzylamine phenylenediamine are added and treated with a stirring speed of 400 r / min for 60 min to obtain slurry.

[0071] The slurry was coated onto the surface of the alumina-based fiber layer with a coating thickness of 3 mm, and then dried at 125°C for 2 hours to obtain welding fireproof cotton.

[0072] Comparative Example 1:

[0073] The difference between Comparative Example 1 and Example 3 is that Comparative Example 1 uses magnesium hydroxide as a single flame retardant, while the rest is the same as Example 3.

[0074] Comparative Example 2:

[0075] The difference between Comparative Example 2 and Example 3 is that Comparative Example 2 uses a single phosphorus-doped biochar as a flame retardant, while the rest is the same as Example 3.

[0076] Comparative Example 3:

[0077] The difference between Comparative Example 3 and Example 3 is that the flame retardant in Comparative Example 3 is obtained by mixing magnesium hydroxide and biochar in a mass ratio of 3:1, while the rest is the same as in Example 3.

[0078] Comparative Example 4:

[0079] The difference between Comparative Example 4 and Example 3 is that no flame retardant was added in Comparative Example 4, but otherwise it was the same as Example 3.

[0080] Comparative Example 5:

[0081] The difference between Comparative Example 5 and Example 3 is that Comparative Example 5 uses a single type of ceramic fiber, while the rest is the same as Example 3.

[0082] Comparative Example 6:

[0083] The difference between Comparative Example 6 and Example 3 is that Comparative Example 6 uses a single type of glass fiber, while the rest is the same as Example 3.

[0084] Comparative Example 7:

[0085] The difference between Comparative Example 7 and Example 3 is that Comparative Example 7 uses a single type of aluminum silicate fiber, while the rest is the same as Example 3.

[0086] Comparative Example 8:

[0087] The difference between Comparative Example 8 and Example 3 is that no modified perlite powder was added in Comparative Example 8, while the rest is the same as in Example 3.

[0088] Comparative Example 9:

[0089] The difference between Comparative Example 9 and Example 3 is that the perlite powder in Comparative Example 9 was not modified, while the rest was the same as in Example 3.

[0090] The samples from Examples 1-3 and the comparative samples from Comparative Examples 1-9 were subjected to performance tests. The fire resistance test was conducted according to GB / T9978.1-2018 "Fire Resistance Test Method for Building Components". The fire resistance duration refers to the product's ability to withstand a corresponding fire exposure time without exceeding the temperature limit on the unexposed surface or losing its integrity during the fire exposure. The results are shown in Table 1 below.

[0091] Table 1: Performance Test Results

[0092]

[0093]

[0094] As can be seen from the data analysis in Table 1, this application improves the fire resistance of the system by optimizing the composition of the flame retardant. Both the biochar and perlite powder are treated, and the phosphorus element is introduced into the biochar and perlite powder after treatment, which further improves the high temperature resistance and fire resistance. The added magnesium hydroxide, phosphorus-doped biochar, modified perlite powder and composite fiber have a synergistic effect, which makes the fireproof cotton prepared by the formula have more significant fire resistance.

[0095] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0096] The embodiments described above are merely illustrative of several implementations of the present invention, and while the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the invention patent. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these all fall within the protection scope of the present invention. Therefore, the protection scope of this invention patent should be determined by the appended claims.

Claims

1. A type of welding fireproof cotton, characterized in that, The welding fireproof cotton includes a base layer and a fireproof layer wrapped around the surface of the base layer, and the fireproof layer comprises the following raw materials by weight: The composition includes 35-38 parts polyester resin, 9-11 parts nano silica, 3-5 parts hydroxypropyl cellulose, 1-7 parts composite fiber, 3-9 parts flame retardant, 3-9 parts modified perlite powder, 1-5 parts antioxidant, 1-2 parts dispersant, 1-2 parts defoamer, 1-3 parts leveling agent, and 10-15 parts water. The flame retardant is obtained by mixing magnesium hydroxide and phosphorus-doped biochar in a mass ratio of (1~3):(1~2). The composite fiber is obtained by mixing ceramic fiber, glass fiber and aluminosilicate fiber in a mass ratio of (1~5):(1~3):(1~9).

2. The welding fireproof cotton according to claim 1, characterized in that, The acid value of the polyester resin is a carboxyl polyester resin between 60 mg KOH / g and 80 mg KOH / g.

3. The welding fireproof cotton according to claim 1, characterized in that, The modified perlite powder is prepared by heat-treating the perlite powder at 250℃~350℃ for 15min~30min, then cooling it to 60℃~65℃, adding a phosphoric acid solution with pH 5.5, stirring for 20min~30min, then adding a silane coupling agent solution, continuing to stir for 15min~30min, washing with water, and drying to obtain the modified perlite powder.

4. The welding fireproof cotton according to claim 3, characterized in that, The phosphoric acid solution has a mass percentage concentration of 5% to 15%, and the silane coupling agent solution has a mass percentage concentration of 3% to 10%.

5. The welding fireproof cotton according to claim 1, characterized in that, The preparation method of the phosphorus-doped biochar is as follows: place the biochar in a phytic acid solution, mix evenly, then heat treat at 250℃~300℃ for 3h~5h, cool to room temperature, and dry to obtain phosphorus-doped biochar.

6. The welding fireproof cotton according to claim 5, characterized in that, The phytic acid solution has a mass percentage concentration of 10% to 15%.

7. The welding fireproof cotton according to claim 1, characterized in that, The substrate layer is an alumina-based fiber layer.

8. The welding fireproof cotton according to claim 1, characterized in that, The antioxidant is at least one of N-benzylamine phenylenediamine and N,N-diphenyl-p-phenylenediamine.

9. A method for preparing welding fireproof cotton, characterized in that, The preparation method is used to prepare the welding fireproof cotton as described in any one of claims 1 to 8, and the preparation method includes the following steps: Polyester resin, nano silica, hydroxypropyl cellulose, composite fiber, dispersant, defoamer, leveling agent and water are added to a reaction vessel, heated to 65℃~85℃, and treated with a stirring speed of 200r / min~300r / min for 30min~40min. Then flame retardant, modified perlite powder and antioxidant are added, and treated with a stirring speed of 350r / min~500r / min for 50min~60min to obtain slurry. The slurry is coated onto the surface of the substrate layer and dried to obtain welding fireproof cotton.

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