A fireproof artificial composite board and preparation method thereof
By using modified resins and modified fillers and other materials, a non-toxic and dripping fire-resistant artificial composite board was prepared, which solved the problem of general flame retardant effect of artificial composite boards in the prior art, and achieved excellent flame retardant effect and security.
Patent Information
- Application Number
- CN202311851184.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-12-29
- Publication Date
- 2025-02-07
- Estimated Expiration
- 2043-12-29
AI Technical Summary
At this stage, the flame retardant effect of artificial composite panels is average, and halogen flame retardant will produce harmful gases during combustion, causing secondary damage.
Fire-resistant artificial composite boards are prepared through specific process steps using raw materials such as straw powder, quartz sand, mica powder, modified resin and modified filler. The modified resin is prepared by the reaction of phosphorus oxychloride and pentaerythritol, and the modified filler is prepared by the reaction of phenylphosphoric acid and magnesium hydroxide and the addition of graphene oxide.
It achieves excellent flame retardant effect that is non-toxic and dripping, reduces the generation of harmful gases, and enhances the flame retardant performance of the material.
Smart Images

Figure BDA0004641056320000101
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of composite board preparation, and in particular to a fireproof artificial composite board and a preparation method thereof. Background Art
[0002] Home decoration and office decoration are becoming increasingly popular. At present, wood boards, gypsum boards or artificial composite boards are generally used for decoration in the market. Wood boards are easy to catch fire and pose a safety hazard. Gypsum boards will fall off after long-term use and have poor moisture resistance. Artificial composite boards have gradually occupied the market due to their excellent service life and good moisture resistance. Artificial boards are mostly made of wood chips and organic resins. The addition of wood chips reduces the flame retardancy of artificial boards. In order to improve their flame retardancy, flame retardants are often added during the preparation of the boards to achieve flame retardant effects. Halogen flame retardants will produce a large amount of harmful gases during combustion. These harmful gases will cause secondary injuries to people during escape and rescue. In severe cases, they will also cause suffocation and death. Therefore, flame retardant materials that can reduce the generation of harmful gases and have excellent flame retardant effects and non-toxic and dripping have become a research hotspot for artificial composite boards. Summary of the invention
[0003] The purpose of the present invention is to provide a fireproof artificial composite board and a preparation method thereof, which solves the problem that the flame retardant effect of the artificial composite board at present is mediocre.
[0004] The purpose of the present invention can be achieved by the following technical solutions:
[0005] A method for preparing a fireproof artificial composite board comprises the following steps:
[0006] Weigh the following raw materials in parts by weight: 8-10 parts of straw powder, 10-15 parts of quartz sand, 5-10 parts of mica powder, 50-60 parts of modified resin, 10-15 parts of modified filler and 5-8 parts of meta-phenylenediamine, mix the raw materials evenly, pour them into a mold, and cure them at a temperature of 150-160° C. to obtain a fireproof artificial composite board.
[0007] Further, the modified resin is prepared by the following steps:
[0008] Step A1: Phosphorus oxychloride, pentaerythritol and DMF are mixed uniformly, reacted at a speed of 60-80 r / min and a temperature of 110-115° C. for 7-9 hours, DMF is removed by distillation, the substrate and formic acid are mixed, nitrogen is introduced for protection, and the reaction is carried out at a temperature of 30-40° C. for 1-1.5 hours to obtain intermediate 1;
[0009] Step A2: The intermediate 1 and DMF are mixed evenly, nitrogen is introduced for protection, 4-vinylphenol is added under stirring at a speed of 120-150 r / min and a temperature of 65-70° C., and the mixture is reacted for 45-50 hours to obtain a modified monomer;
[0010] Step A3: uniformly mix the modified monomer, epichlorohydrin and DMF, react for 3-5 hours at a rotation speed of 120-150 r / min and a temperature of 100-105° C., then cool to 70-75° C., add sodium hydroxide solution, and react for 5-7 hours to obtain a modified resin.
[0011] Furthermore, the molar ratio of phosphorus oxychloride, pentaerythritol and formic acid in step A1 is 2:1:2.
[0012] Furthermore, the molar ratio of the intermediate 1 and 4-vinylphenol described in step A2 is 1:2.
[0013] Furthermore, the amount ratio of the modified monomer, epichlorohydrin and sodium hydroxide solution described in step A3 is 1 mmol:10 mmol:10 mL, and the mass fraction of the sodium hydroxide solution is 1.5%.
[0014] Further, the modified filler is prepared by the following steps:
[0015] Step B1: dissolving phenyl phosphate in ethanol, stirring and adding magnesium hydroxide at a speed of 120-150 r / min and a temperature of 60-65° C., heating to 80-85° C., reflux reaction for 5-7 hours, adding graphene oxide and deionized water, heating to 90-95° C., reacting for 8-10 hours, filtering and removing the filtrate to obtain modified graphene, and uniformly mixing the modified graphene, KH550, DCC and DMF, reacting for 3-5 hours at a speed of 200-300 r / min and a temperature of 30-40° C. to obtain a precursor;
[0016] Step B2: 4-formylphenylboronic acid, pentaerythritol and DMF are mixed uniformly, and boron trichloride is added under stirring at a speed of 200-300 r / min and a temperature of 80-100° C., and the mixture is reacted for 6-8 hours to obtain intermediate 2; intermediate 2, KH550 and ethanol are mixed uniformly, and nitrogen is introduced for protection, and the mixture is reacted at a speed of 150-200 r / min and a temperature of 50-60° C. for 3-5 hours to obtain intermediate 3;
[0017] Step B3: The intermediate 3 and ethanol are mixed evenly, nitrogen protection is introduced, DOPO is added under stirring at a speed of 120-150 r / min and a temperature of 80-85°C, and the reaction is carried out for 3-5 hours to obtain the intermediate 4. The precursor, intermediate 4, KH550 and DMF are mixed evenly, deionized water is added under stirring at a speed of 120-150 r / min and a temperature of 60-70°C, and the reaction is carried out for 10-15 hours, then the temperature is lowered to room temperature, ammonium fluoride is added, the reaction is continued for 20-25 hours, the temperature is raised to 80-85°C, and the temperature is aged for 7-9 days to obtain the modified filler.
[0018] Furthermore, the amount ratio of phenylphosphoric acid, magnesium hydroxide, graphene oxide and deionized water in step B1 is 15g:1g:1g:200mL, and the amount ratio of modified graphene, KH550 and DCC is 1g:10mmo l:10mmo l.
[0019] Furthermore, the molar ratio of 4-formylphenylboronic acid and pentaerythritol in step B2 is 2:1, the amount of boron trichloride used is 1-1.5% of the mass of 4-formylphenylboronic acid and pentaerythritol, and the molar ratio of intermediate 2 and KH550 is 1:2.
[0020] Furthermore, the molar ratio of the intermediate 3 and DOPO in step B3 is 1:2, and the amount ratio of the precursor, the intermediate 4, KH550 and ammonium fluoride is 1g:20mmol:3mL:3g.
[0021] Beneficial effects of the present invention: A fireproof artificial composite board prepared by the present invention comprises the following raw materials: straw powder, quartz sand, mica powder, modified resin, modified filler and m-phenylenediamine; the modified resin uses phosphorus oxychloride and pentaerythritol as raw materials, so that two chlorine atom sites on the phosphorus oxychloride react with two hydroxyl groups on the pentaerythritol, and under the action of formic acid, the P-Cl bond is converted into a PH bond to obtain an intermediate 1; the intermediate 1 is reacted with 4-vinylphenol, so that the PH bond on the intermediate 1 reacts with the vinyl on the 4-vinylphenol to obtain a modified monomer; and the modified The modified resin is prepared by reacting the monomer with epichlorohydrin to form an epoxy resin. The modified resin contains an organic phosphorus structure. During the combustion process, the organic phosphorus can be carbonized and coated on the surface of the material, thereby isolating the combustible gas from contacting the combustion site, and at the same time, it can insulate heat to achieve a flame retardant effect. The modified filler is dehydrated with phenylphosphoric acid and magnesium hydroxide to form an organic-inorganic symmetrical hybrid structure, and then graphene oxide is added to make part of the carboxyl groups on the graphene oxide react with P-OH to prepare modified graphene. The modified graphene is reacted with KH550 under the action of DCC to make the modified The remaining carboxyl groups on the graphene react with the amino groups on KH550 by dehydration to obtain a precursor, 4-formylphenylboronic acid reacts with pentaerythritol, so that the boronic acid group on 4-formylphenylboronic acid reacts with the hydroxyl group on pentaerythritol to obtain intermediate 2, intermediate 2 reacts with KH550, so that the aldehyde group on intermediate 2 reacts with the amino group on KH550 to form a C=N bond to obtain intermediate 3, intermediate 3 reacts with DOPO, so that the C=N bond on intermediate 3 reacts with the PH on DOPO to obtain intermediate 4, and the precursor and intermediate 4 are reacted. The modified filler is hydrolyzed and condensed with KH550 to form an amino cage-type silsesquioxane between the precursor and the intermediate 4 to obtain a modified filler. During combustion, the magnesium on the modified filler can form magnesium oxide, thereby densifying the carbon layer produced by the polyphosphate and reducing the generation of smoke. At the same time, the modified filler contains a large amount of Si-O bonds, N elements and P elements. The Si-O bonds generate Si-C bonds during combustion. The N elements and P elements can further stabilize the carbon layer and enhance the flame retardant effect. The surface of the modified filler contains active amino groups that can participate in the curing of the modified resin and enhance the flame retardant effect. DETAILED DESCRIPTION
[0022] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0023] Example 1
[0024] A method for preparing a fireproof artificial composite board comprises the following steps:
[0025] Weigh the following raw materials in parts by weight: 8 parts of straw powder, 10 parts of quartz sand, 5 parts of mica powder, 50 parts of modified resin, 10 parts of modified filler and 5 parts of meta-phenylenediamine, mix the raw materials evenly, pour them into a mold, and cure them at a temperature of 150° C. to obtain a fireproof artificial composite board.
[0026] The modified resin is prepared by the following steps:
[0027] Step A1: Phosphorus oxychloride, pentaerythritol and DMF are mixed evenly, reacted at a speed of 60 r / min and a temperature of 110° C. for 7 h, DMF is distilled off, the substrate and formic acid are mixed, nitrogen is introduced for protection, and the reaction is carried out at a temperature of 30° C. for 1 h to obtain intermediate 1;
[0028] Step A2: The intermediate 1 and DMF were mixed evenly, nitrogen was introduced for protection, 4-vinylphenol was added under stirring at a speed of 120 r / min and a temperature of 65° C., and the mixture was reacted for 45 h to obtain a modified monomer;
[0029] Step A3: The modified monomer, epichlorohydrin and DMF were mixed evenly, reacted at a speed of 120 r / min and a temperature of 100° C. for 3 h, then cooled to 70° C., sodium hydroxide solution was added, and reacted for 5 h to obtain a modified resin.
[0030] The molar ratio of phosphorus oxychloride, pentaerythritol and formic acid in step A1 is 2:1:2.
[0031] The molar ratio of the intermediate 1 and 4-vinylphenol in step A2 is 1:2.
[0032] The amount ratio of the modified monomer, epichlorohydrin and sodium hydroxide solution described in step A3 is 1 mmol:10 mmol:10 mL, and the mass fraction of the sodium hydroxide solution is 1.5%.
[0033] The modified filler is prepared by the following steps:
[0034] Step B1: dissolving phenyl phosphate in ethanol, stirring and adding magnesium hydroxide at a speed of 120 r / min and a temperature of 60°C, heating to 80°C, reflux reaction for 5 hours, adding graphene oxide and deionized water, heating to 90°C, reacting for 8 hours, filtering and removing the filtrate to obtain modified graphene, and uniformly mixing the modified graphene, KH550, DCC and DMF, reacting for 3 hours at a speed of 200 r / min and a temperature of 30°C to obtain a precursor;
[0035] Step B2: 4-formylphenylboronic acid, pentaerythritol and DMF were mixed evenly, and boron trichloride was added under stirring at a speed of 200 r / min and a temperature of 80°C, and the reaction was carried out for 6 hours to obtain intermediate 2; intermediate 2, KH550 and ethanol were mixed evenly, and nitrogen was introduced for protection, and the reaction was carried out at a speed of 150 r / min and a temperature of 50°C for 3 hours to obtain intermediate 3;
[0036] Step B3: The intermediate 3 and ethanol were mixed evenly, nitrogen was introduced for protection, DOPO was added under stirring at a speed of 120 r / min and a temperature of 80°C, and the reaction was carried out for 3 hours to obtain the intermediate 4. The precursor, intermediate 4, KH550 and DMF were mixed evenly, deionized water was added under stirring at a speed of 120 r / min and a temperature of 60°C, and the reaction was carried out for 10 hours. The mixture was cooled to room temperature, ammonium fluoride was added, the reaction was continued for 20 hours, the temperature was raised to 80°C, and the mixture was aged for 7 days to obtain the modified filler.
[0037] The amount ratio of phenylphosphoric acid, magnesium hydroxide, graphene oxide and deionized water described in step B1 is 15g:1g:1g:200mL, and the amount ratio of modified graphene, KH550 and DCC is 1g:10mmo l:10mmo l.
[0038] The molar ratio of 4-formylphenylboronic acid and pentaerythritol in step B2 is 2:1, the amount of boron trichloride used is 1% by mass of 4-formylphenylboronic acid and pentaerythritol, and the molar ratio of intermediate 2 and KH550 is 1:2.
[0039] The molar ratio of intermediate 3 and DOPO in step B3 is 1:2, and the usage ratio of precursor, intermediate 4, KH550 and ammonium fluoride is 1 g:20 mmol:3 mL:3 g.
[0040] Example 2
[0041] A method for preparing a fireproof artificial composite board comprises the following steps:
[0042] Weigh the following raw materials in parts by weight: 9 parts of straw powder, 13 parts of quartz sand, 8 parts of mica powder, 55 parts of modified resin, 13 parts of modified filler and 6 parts of meta-phenylenediamine, mix the raw materials evenly, pour them into a mold, and cure them at a temperature of 155° C. to obtain a fireproof artificial composite board.
[0043] The modified resin is prepared by the following steps:
[0044] Step A1: Phosphorus oxychloride, pentaerythritol and DMF are mixed evenly, reacted at a speed of 60 r / min and a temperature of 115° C. for 8 h, DMF is distilled off, the substrate and formic acid are mixed, nitrogen is introduced for protection, and the reaction is carried out at a temperature of 35° C. for 1.5 h to obtain intermediate 1;
[0045] Step A2: The intermediate 1 and DMF were mixed evenly, nitrogen was introduced for protection, 4-vinylphenol was added under stirring at a speed of 120 r / min and a temperature of 68° C., and the mixture was reacted for 48 hours to obtain a modified monomer;
[0046] Step A3: The modified monomer, epichlorohydrin and DMF were mixed evenly, reacted at a speed of 150 r / min and a temperature of 100° C. for 4 hours, then cooled to 73° C., sodium hydroxide solution was added, and reacted for 6 hours to obtain a modified resin.
[0047] The molar ratio of phosphorus oxychloride, pentaerythritol and formic acid in step A1 is 2:1:2.
[0048] The molar ratio of the intermediate 1 and 4-vinylphenol in step A2 is 1:2.
[0049] The amount ratio of the modified monomer, epichlorohydrin and sodium hydroxide solution described in step A3 is 1 mmol:10 mmol:10 mL, and the mass fraction of the sodium hydroxide solution is 1.5%.
[0050] The modified filler is prepared by the following steps:
[0051] Step B1: dissolving phenyl phosphate in ethanol, stirring and adding magnesium hydroxide at a speed of 150 r / min and a temperature of 60° C., heating to 83° C., reflux reaction for 6 hours, adding graphene oxide and deionized water, heating to 93° C., reacting for 9 hours, filtering and removing the filtrate to obtain modified graphene, and uniformly mixing the modified graphene, KH550, DCC and DMF, reacting for 4 hours at a speed of 200 r / min and a temperature of 35° C. to obtain a precursor;
[0052] Step B2: 4-formylphenylboronic acid, pentaerythritol and DMF were mixed evenly, and boron trichloride was added under stirring at a speed of 200 r / min and a temperature of 90°C, and the reaction was carried out for 7 hours to obtain intermediate 2; intermediate 2, KH550 and ethanol were mixed evenly, and nitrogen was introduced for protection, and the reaction was carried out at a speed of 150 r / min and a temperature of 55°C for 4 hours to obtain intermediate 3;
[0053] Step B3: The intermediate 3 and ethanol were mixed evenly, nitrogen was introduced for protection, DOPO was added under stirring at a speed of 120 r / min and a temperature of 85°C, and the reaction was carried out for 4 hours to obtain the intermediate 4. The precursor, intermediate 4, KH550 and DMF were mixed evenly, deionized water was added under stirring at a speed of 120 r / min and a temperature of 65°C, and the reaction was carried out for 15 hours. The mixture was cooled to room temperature, ammonium fluoride was added, the reaction was continued for 23 hours, the temperature was raised to 83°C, and the mixture was aged for 8 days to obtain the modified filler.
[0054] The amount ratio of phenylphosphoric acid, magnesium hydroxide, graphene oxide and deionized water described in step B1 is 15g:1g:1g:200mL, and the amount ratio of modified graphene, KH550 and DCC is 1g:10mmo l:10mmo l.
[0055] The molar ratio of 4-formylphenylboronic acid and pentaerythritol in step B2 is 2:1, the amount of boron trichloride used is 1-1.5% of the mass of 4-formylphenylboronic acid and pentaerythritol, and the molar ratio of intermediate 2 and KH550 is 1:2.
[0056] The molar ratio of intermediate 3 and DOPO in step B3 is 1:2, and the usage ratio of precursor, intermediate 4, KH550 and ammonium fluoride is 1 g:20 mmol:3 mL:3 g.
[0057] Example 3
[0058] A method for preparing a fireproof artificial composite board comprises the following steps:
[0059] Weigh the following raw materials in parts by weight: 10 parts of straw powder, 15 parts of quartz sand, 10 parts of mica powder, 60 parts of modified resin, 15 parts of modified filler and 8 parts of meta-phenylenediamine, mix the raw materials evenly, pour them into a mold, and cure them at a temperature of 160° C. to obtain a fireproof artificial composite board.
[0060] The modified resin is prepared by the following steps:
[0061] Step A1: Phosphorus oxychloride, pentaerythritol and DMF are mixed evenly, and reacted at a speed of 80 r / min and a temperature of 115° C. for 9 h, and DMF is distilled off. The substrate and formic acid are mixed, and nitrogen is introduced for protection, and the reaction is carried out at a temperature of 40° C. for 1.5 h to obtain intermediate 1;
[0062] Step A2: The intermediate 1 and DMF were mixed evenly, nitrogen was introduced for protection, 4-vinylphenol was added under stirring at a speed of 150 r / min and a temperature of 70° C., and the mixture was reacted for 50 h to obtain a modified monomer;
[0063] Step A3: The modified monomer, epichlorohydrin and DMF were mixed evenly, reacted at a speed of 150 r / min and a temperature of 105° C. for 5 hours, then cooled to 75° C., sodium hydroxide solution was added, and reacted for 7 hours to obtain a modified resin.
[0064] The molar ratio of phosphorus oxychloride, pentaerythritol and formic acid in step A1 is 2:1:2.
[0065] The molar ratio of the intermediate 1 and 4-vinylphenol in step A2 is 1:2.
[0066] The amount ratio of the modified monomer, epichlorohydrin and sodium hydroxide solution described in step A3 is 1 mmol:10 mmol:10 mL, and the mass fraction of the sodium hydroxide solution is 1.5%.
[0067] The modified filler is prepared by the following steps:
[0068] Step B1: dissolving phenyl phosphate in ethanol, stirring and adding magnesium hydroxide at a speed of 150 r / min and a temperature of 65°C, heating to 85°C, reflux reaction for 7 hours, adding graphene oxide and deionized water, heating to 95°C, reacting for 10 hours, filtering and removing the filtrate to obtain modified graphene, and uniformly mixing the modified graphene, KH550, DCC and DMF, reacting for 5 hours at a speed of 300 r / min and a temperature of 40°C to obtain a precursor;
[0069] Step B2: 4-formylphenylboronic acid, pentaerythritol and DMF were mixed evenly, and boron trichloride was added under stirring at a speed of 300 r / min and a temperature of 100° C., and the mixture was reacted for 8 h to obtain intermediate 2; intermediate 2, KH550 and ethanol were mixed evenly, and nitrogen was introduced for protection, and the mixture was reacted at a speed of 200 r / min and a temperature of 60° C. for 5 h to obtain intermediate 3;
[0070] Step B3: The intermediate 3 and ethanol were mixed evenly, nitrogen was introduced for protection, DOPO was added under stirring at a speed of 150 r / min and a temperature of 85°C, and the reaction was carried out for 5 hours to obtain the intermediate 4. The precursor, intermediate 4, KH550 and DMF were mixed evenly, deionized water was added under stirring at a speed of 150 r / min and a temperature of 70°C, and the reaction was carried out for 15 hours. The mixture was cooled to room temperature, ammonium fluoride was added, the reaction was continued for 25 hours, the temperature was raised to 85°C, and the mixture was aged for 9 days to obtain the modified filler.
[0071] The amount ratio of phenylphosphoric acid, magnesium hydroxide, graphene oxide and deionized water described in step B1 is 15g:1g:1g:200mL, and the amount ratio of modified graphene, KH550 and DCC is 1g:10mmo l:10mmo l.
[0072] The molar ratio of 4-formylphenylboronic acid and pentaerythritol in step B2 is 2:1, the amount of boron trichloride used is 1.5% of the mass of 4-formylphenylboronic acid and pentaerythritol, and the molar ratio of intermediate 2 and KH550 is 1:2.
[0073] The molar ratio of intermediate 3 and DOPO in step B3 is 1:2, and the usage ratio of precursor, intermediate 4, KH550 and ammonium fluoride is 1 g:20 mmol:3 mL:3 g.
[0074] Comparative Example 1
[0075] Compared with Example 1, no modified filler was added in this comparative example, and the remaining steps were the same.
[0076] Comparative Example 2
[0077] Compared with Example 1, this comparative example uses a precursor instead of a modified filler, and the remaining steps are the same.
[0078] Comparative Example 3
[0079] Compared with Example 1, this comparative example uses graphene oxide instead of modified graphene, and the remaining steps are the same.
[0080] The sheath materials prepared in Examples 1-3 and Comparative Examples 1-3 were tested for combustion grade according to ASTM 635-2003, with the sample size being 130 mm × 15 mm × 5 mm, and for limiting oxygen index according to GB / T20462-2008, with the sample size being 130 mm × 10 mm × 5 mm. The test results are shown in the following table.
[0081]
[0082] It can be seen from the above table that this application has a very good flame retardant effect.
[0083] The above contents are merely examples and explanations of the concept of the present invention. The technicians in this technical field may make various modifications or additions to the specific embodiments described or replace them in a similar manner. As long as they do not deviate from the concept of the invention or exceed the scope defined by the claims, they should all fall within the protection scope of the present invention.
Claims
1. A method for preparing a fireproof artificial composite board, characterized in that: The specific steps include: Weigh the following raw materials by weight: 8-10 parts of straw powder, 10-15 parts of quartz sand, 5-10 parts of mica powder, 50-60 parts of modified resin, 10-15 parts of modified filler and 5-8 parts of m-phenylenediamine, mix the raw materials evenly, pour them into a mold, and cure them at a temperature of 150-160° C. to obtain a fireproof artificial composite board; The modified resin is prepared by the following steps: Step A1: phosphorus oxychloride, pentaerythritol and DMF are mixed for reaction, DMF is removed by distillation, the substrate and formic acid are mixed, nitrogen is introduced for protection, and the reaction is carried out to obtain intermediate 1; Step A2: The intermediate 1 and DMF are uniformly mixed, nitrogen is introduced for protection, 4-vinylphenol is added and stirred, and a reaction is carried out to obtain a modified monomer; Step A3: After the modified monomer, epichlorohydrin and DMF are mixed and reacted, a sodium hydroxide solution is added and the reaction is continued to obtain a modified resin; The modified filler is prepared by the following steps: Step B1: dissolving phenyl phosphate in ethanol, stirring and adding magnesium hydroxide, heating and refluxing to react, adding graphene oxide and deionized water, heating and continuing the reaction, filtering and removing the filtrate to obtain modified graphene, and mixing the modified graphene, KH550, DCC and DMF to react to obtain a precursor; Step B2: 4-formylphenylboronic acid, pentaerythritol and DMF were mixed and stirred, and boron trichloride was added to react to obtain intermediate 2; intermediate 2, KH550 and ethanol were mixed evenly, and nitrogen was introduced for protection to react to obtain intermediate 3; Step B3: The intermediate 3 and ethanol are mixed evenly, nitrogen is introduced for protection, DOPO is added after stirring, and the reaction is carried out to obtain the intermediate 4. The precursor, the intermediate 4, KH550 and DMF are mixed and stirred, and deionized water is added. After the reaction, the temperature is lowered to room temperature, ammonium fluoride is added, the reaction is continued, and the temperature is raised for aging to obtain the modified filler.
2. The method for preparing a fireproof artificial composite board according to claim 1, characterized in that: The molar ratio of phosphorus oxychloride, pentaerythritol and formic acid in step A1 is 2:1:
2.
3. The method for preparing a fireproof artificial composite board according to claim 1, characterized in that: The molar ratio of the intermediate 1 and 4-vinylphenol in step A2 is 1:
2.
4. The method for preparing a fireproof artificial composite board according to claim 1, characterized in that: The amount ratio of the modified monomer, epichlorohydrin and sodium hydroxide solution described in step A3 is 1 mmol:10 mmol:10 mL, and the mass fraction of the sodium hydroxide solution is 1.5%.
5. The method for preparing a fireproof artificial composite board according to claim 1, characterized in that: The amount ratio of phenylphosphoric acid, magnesium hydroxide, graphene oxide and deionized water described in step B1 is 15g:1g:1g:200mL, and the amount ratio of modified graphene, KH550 and DCC is 1g:10mmol:10mmol.
6. The method for preparing a fireproof artificial composite board according to claim 1, characterized in that: The molar ratio of 4-formylphenylboronic acid and pentaerythritol in step B2 is 2:1, the amount of boron trichloride used is 1-1.5% of the mass of 4-formylphenylboronic acid and pentaerythritol, and the molar ratio of intermediate 2 and KH550 is 1:
2.
7. The method for preparing a fireproof artificial composite board according to claim 1, characterized in that: The molar ratio of intermediate 3 and DOPO described in step B3 is 1:2, and the amount ratio of precursor, intermediate 4, KH550 and ammonium fluoride is 1g:20mmol:3mL:3g.
8. A fireproof artificial composite board, characterized in that: Prepared according to any one of claims 1 to 7.
Citation Information
Patent Citations
Electric flame-retardant partition plate and preparation process thereof
CN113429708A