Graphene flame-retardant polyester fiberboard

Abstract

The application discloses a graphene flame-retardant polyester fiber plate, which comprises polyester fibers, modified graphene agents, flame retardants and coordination treatment liquid, and the mass ratio of the polyester fibers, the modified graphene agents, the flame retardants and the coordination treatment liquid is (9-11):(3-5):0.5:(13-15). The graphene flame-retardant polyester fiber plate adopts polyester fibers as a matrix, and the performance coordination of the product is optimized by the modified graphene agents and the coordination treatment liquid. The polyester fibers are first sent into the coordination treatment liquid for primary stirring and modification, and then are added with the modified graphene agents for secondary modification and optimization. The flame-retardant and sound-absorbing performance of the product is improved through the coordination effect among raw materials.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of polyester fiber board, in particular to a graphene flame-retardant polyester fiber board. BACKGROUND

[0002] The polyester fiber sound absorption board, also known as glass wool, is a material with sound absorption function made of polyester fiber as raw material by hot pressing. It is generally used in engineering noise reduction: automobile engine, engineering motor sealing to relieve noise. It has good effect on high frequency and high decibel noise.

[0003] The existing polyester fiber board has sound absorption effect, but the flame retardance is poor. In order to improve the flame retardance of the product, the sound absorption effect of the product is reduced. Based on this, the present application improves the flame retardance and sound absorption performance, and the performance of the product under acid corrosion is poor, so further improvement is needed. SUMMARY

[0004] In view of the defects of the prior art, the purpose of the present application is to provide a graphene flame-retardant polyester fiber board to solve the problems in the background art.

[0005] The technical problem solved by the present application adopts the following technical scheme:

[0006] The present application provides a graphene flame-retardant polyester fiber board, which comprises polyester fiber, modified graphene agent, flame retardant and coordination treatment liquid, wherein the mass ratio of polyester fiber, modified graphene agent, flame retardant and coordination treatment liquid is (9-11):(3-5):0.5:(13-15).

[0007] The preparation method of the flame-retardant polyester fiber board is as follows:

[0008] Step one: first, the polyester fiber is sent into the coordination treatment liquid for primary stirring modification treatment;

[0009] Step two: preparation of modified graphene agent;

[0010] Step three: then the modified graphene agent and tributyl phosphate flame retardant are added to the product of step one for secondary stirring modification treatment;

[0011] Step four: then open the treatment and card into a net, cross-lay after needle punching reinforcement, hot air reinforcement in the oven at 180 DEG C;

[0012] Step five: the product of step four is placed in a hot press at 0.5-0.7 MPa and 125 DEG C to form a graphene flame-retardant polyester fiber board.

[0013] Preferably, the preparation of the modified graphene agent is as follows:

[0014] S01, the graphene is added into the hydrochloric acid solution in a weight ratio of 1:6, stirred uniformly, then 2-5% of lanthanum sulfate and 1-5% of alkyl sulfonate sodium of the total amount of graphene are added, stirred fully, then washed with water and dried;

[0015] S02, 5-10% of the ball milling modifier of the total amount of S01 product is added into the product of S01, ball milling modification is performed, the rotation speed of ball milling modification is 1150-1250 r / min, the ball milling time is 40-50 min, after ball milling, washing with water and drying, the modified graphene agent is obtained.

[0016] Preferably, the mass fraction of the hydrochloric acid solution is 3-6%.

[0017] Preferably, the ball milling modifier comprises the following raw materials by weight:

[0018] 3-6 parts of carboxymethyl cellulose, 10-15 parts of chitosan aqueous solution, 1-3 parts of phosphate buffer solution, 2-5 parts of hydroxyapatite and 0.2-0.5 parts of barium titanate.

[0019] Preferably, the mass fraction of the chitosan aqueous solution is 6-10%, and the pH value of the phosphate buffer solution is 5.0.

[0020] Preferably, the rotation speed of the primary stirring modification treatment is 350-450 r / min, the stirring time is 30-40 min, and the stirring temperature is 40-45℃.

[0021] Preferably, the rotation speed of the primary stirring modification treatment is 800-1200 r / min, the stirring time is 10-20 min, and the stirring temperature is 46-48℃.

[0022] Preferably, the preparation method of the coordination treatment liquid is as follows:

[0023] S101: the silicon carbide whisker is heat treated at 140-150℃ for 5-10 min, then heated to 210-220℃ at a rate of 1-3℃ / min, kept for 10-20 min, then decreased to 40-45℃ at a rate of 3-5℃ / min;

[0024] S102: the bentonite is sent into 3-5 times of ethanol solvent, stirred and dispersed uniformly to obtain a bentonite suspension; 1-4 parts of silane coupling agent, 1-3 parts of Tween 60 and 5-10 parts of tetra-n-propyl zirconate are added into 15-25 parts of the bentonite suspension, stirred fully, then washed with water and dried to obtain a bentonite coordination agent;

[0025] S103: the bentonite coordination agent is sent into 5-10 times of deionized water, stirred uniformly, then 2-5% of sodium alginate and 1-5% of sodium dodecyl sulfate of the total amount of bentonite are added, stirred fully to obtain an adjusted bentonite liquid.

[0026] S104: Then the product of S101 is placed in 3-5 times of the adjusted bentonite liquid for ultrasonic dispersion, to obtain a coordinated treatment liquid.

[0027] Preferably, the power of the ultrasonic dispersion is 350-400W, and the ultrasonic time is 20-30min.

[0028] Preferably, the silane coupling agent is silane coupling agent KH560.

[0029] Compared with the prior art, the present application has the following beneficial effects:

[0030] The graphene flame-retardant polyester fiber board of the present application adopts polyester fiber as the matrix, and the performance coordination of the product is optimized by modifying graphene agent and coordinating treatment liquid. The polyester fiber is first sent into the coordinated treatment liquid for primary stirring modification, and then added with modified graphene agent for secondary modification and optimization. Through the coordination effect between raw materials, the flame-retardant and sound-absorbing performance of the product is improved and coordinated, and the product is stable under acid corrosion conditions. The silicon carbide crystal is heat-treated at 140-150℃ for 5-10min, then heated to 210-220℃ at a rate of 1-3℃ / min, and kept for 10-20min, and then cooled to 40-45℃ at a rate of 3-5℃ / min. Through different temperature treatments, the activity of the whisker is optimized. The bentonite is dispersed by ethanol to improve its dispersity, and then optimized by silane coupling agent, Tween 60 and tetra-n-propyl zirconate. The interface of the bentonite is improved, and then the coordinated treatment liquid formed by sodium alginate and sodium dodecyl sulfate is used. The polyester fiber is better dispersed in the coordinated treatment liquid in the primary stirring modification to improve the uniformity of the matrix distribution. The bentonite has a lamellar structure, and is used with the coordinated treatment liquid optimized by the whisker. Through the matrix effect of the flame retardant, the flame-retardant performance of the matrix is further enhanced. Due to the space accommodation degree of the interlayer gap of the bentonite, the sound-absorbing effect is further enhanced after modification and optimization, so as to coordinate and optimize the flame-retardant and sound-absorbing performance of the product. Through the secondary stirring modification and treatment by adding modified graphene agent, the lamellar activity of the graphene is enhanced after being combined with hydrochloric acid solution and lanthanum sulfate. Then the graphene is ball-milled by a ball-milling modifier. The raw materials in the ball-milling modifier, such as carboxymethyl cellulose, chitosan aqueous solution, phosphate buffer solution, hydroxyapatite and barium titanate, are coordinated and improved to optimize the modified graphene. The prepared modified graphene agent has the effects of reinforcing and coordinating the coordinated treatment liquid, and together improves the flame-retardant and sound-absorbing performance of the product, and optimizes the acid corrosion stability of the product. DETAILED DESCRIPTION

[0031] The technical solutions in the embodiments of the present application will be clearly and completely described below in conjunction with specific embodiments. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative work fall within the scope of the present application.

[0032] The graphene flame-retardant polyester fiber plate in the embodiment comprises polyester fibers, modified graphene agents, flame retardants and coordination treatment liquid, wherein the mass ratio of the polyester fibers, the modified graphene agents, the flame retardants and the coordination treatment liquid is (9-11):(3-5):0.5:(13-15).

[0033] The preparation method of the flame-retardant polyester fiber plate is as follows:

[0034] Step one: first, the polyester fibers are sent into the coordination treatment liquid for primary stirring modification treatment;

[0035] Step two: preparation of the modified graphene agent;

[0036] Step three: then, the modified graphene agent and the tributyl phosphate flame retardant are added to the product of step one for secondary stirring modification treatment;

[0037] Step four: then, after the opening treatment, the product is carded into a web, cross-laid and needle-punched for reinforcement, and then hot air reinforced in an oven at 180 DEG C;

[0038] Step five: the product of step four is placed in a hot press at 0.5-0.7 MPa and 125 DEG C to form a graphene flame-retardant polyester fiber plate.

[0039] Preparation of the modified graphene agent in the embodiment:

[0040] S01: the graphene is added into a hydrochloric acid solution in a weight ratio of 1:6 and stirred uniformly, then 2-5% of lanthanum sulfate and 1-5% of sodium alkyl sulfonate are added, and stirred fully, and then washed with water and dried;

[0041] S02: 5-10% of a ball-milling modifier of the total amount of the product of S01 is added to the product of S01, and then ball-milling modification is performed, the rotation speed of the ball-milling modification is 1150-1250 r / min, the ball-milling time is 40-50 min, and then the product is washed with water and dried to obtain the modified graphene agent.

[0042] The mass fraction of the hydrochloric acid solution in the embodiment is 3-6%.

[0043] The ball-milling modifier in the embodiment comprises the following raw materials by weight:

[0044] 3-6 parts of carboxymethyl cellulose, 10-15 parts of chitosan aqueous solution, 1-3 parts of phosphate buffer solution, 2-5 parts of hydroxyapatite and 0.2-0.5 parts of barium titanate.

[0045] The mass fraction of the chitosan aqueous solution of the embodiment is 6-10%; and the pH value of the phosphate buffer solution is 5.0.

[0046] The rotational speed of the primary stirring modification treatment of the embodiment is 350-450 r / min, the stirring time is 30-40 min, and the stirring temperature is 40-45℃.

[0047] The rotational speed of the primary stirring modification treatment of the embodiment is 800-1200 r / min, the stirring time is 10-20 min, and the stirring temperature is 46-48℃.

[0048] The preparation method of the coordination treatment liquid of the embodiment is as follows:

[0049] S101: heat treating the silicon carbide whisker at 140-150℃ for 5-10 min, then heating to 210-220℃ at a rate of 1-3℃ / min, keeping the temperature for 10-20 min, and then decreasing the temperature to 40-45℃ at a rate of 3-5℃ / min;

[0050] S102: putting the bentonite into 3-5 times of ethanol solvent, stirring and uniformly dispersing to obtain a bentonite suspension; adding 1-4 parts of a silane coupling agent, 1-3 parts of Tween 60 and 5-10 parts of tetra-n-propyl zirconate into 15-25 parts of the bentonite suspension, stirring fully, and finally washing with water and drying to obtain a bentonite coordination agent;

[0051] S103: putting the bentonite coordination agent into 5-10 times of deionized water and stirring uniformly, then adding 2-5% of sodium alginate and 1-5% of sodium dodecyl sulfate based on the total amount of bentonite, stirring fully to obtain an adjusted bentonite liquid;

[0052] S104: then putting the product of S101 into 3-5 times of the adjusted bentonite liquid and ultrasonically dispersing to obtain a coordination treatment liquid.

[0053] The power of the ultrasonic dispersion of the embodiment is 350-400 W, and the ultrasonic time is 20-30 min.

[0054] The silane coupling agent of the embodiment is silane coupling agent KH560.

[0055] Embodiment 1.

[0056] The graphene flame-retardant polyester fiber plate of the embodiment comprises polyester fibers, modified graphene agent, flame retardant, and coordination treatment liquid, wherein the mass ratio of the polyester fibers, modified graphene agent, flame retardant, and coordination treatment liquid is 9:3:0.5:13.

[0057] The preparation method of the flame-retardant polyester fiber plate is as follows:

[0058] Step one: first, the polyester fibers are sent into the coordination treatment liquid for primary stirring modification treatment;

[0059] Step two: preparation of the modified graphene agent;

[0060] Step three: then, the modified graphene agent and tributyl phosphate flame retardant are added to the product of step one for secondary stirring modification treatment;

[0061] Step four: then, after opening treatment, the product is carded into a web, cross-laid, and needle punched for reinforcement, and then hot air reinforcement is performed in an oven at 180℃;

[0062] Step five: the product of step four is placed in a hot press at 0.5MPa and 125℃ to form a graphene flame-retardant polyester fiber plate.

[0063] Preparation of the modified graphene agent of the embodiment:

[0064] S01: the graphene is added into a hydrochloric acid solution in a weight ratio of 1:6 and stirred uniformly, then 2% of lanthanum sulfate and 1% of sodium alkyl sulfonate are added, and the mixture is stirred fully, then washed with water and dried;

[0065] S02: 5% of a ball milling modifier of the total amount of the product of S01 is added to the product of S01, and the mixture is ball milled, the rotation speed of the ball milling modification is 1150r / min, the ball milling time is 40min, and after the ball milling is completed, the mixture is washed with water and dried to obtain the modified graphene agent.

[0066] The mass fraction of the hydrochloric acid solution of the embodiment is 3%.

[0067] The ball milling modifier of the embodiment comprises the following raw materials in parts by weight:

[0068] 3 parts of carboxymethyl cellulose, 10 parts of chitosan aqueous solution, 1 part of phosphate buffer solution, 2 parts of hydroxyapatite, and 0.2 parts of barium titanate.

[0069] The mass fraction of the chitosan aqueous solution of the embodiment is 6%, and the pH value of the phosphate buffer solution is 5.0.

[0070] The rotation speed of the primary stirring modification treatment of the embodiment is 350r / min, the stirring time is 30min, and the stirring temperature is 40℃.

[0071] The rotational speed of the primary stirring modification treatment of this embodiment is 800 r / min, the stirring time is 10 min, and the stirring temperature is 46°C.

[0072] The preparation method of the coordination treatment liquid of this embodiment is as follows:

[0073] S101: heat the silicon carbide whiskers at 140°C for 5 min, then increase the temperature to 210°C at a rate of 1°C / min, keep the temperature for 10 min, and then decrease the temperature to 40°C at a rate of 3°C / min;

[0074] S102: Put the bentonite into 3 times of ethanol solvent and stir to disperse uniformly to obtain a bentonite suspension; add 1 part of a silane coupling agent, 1 part of Tween 60, and 5 parts of tetra-n-propyl zirconate into 15 parts of the bentonite suspension and stir thoroughly, and then wash with water and dry to obtain a bentonite coordination agent;

[0075] S103: Put the bentonite coordination agent into 5 times of deionized water and stir uniformly, then add 2% of sodium alginate and 1% of sodium dodecyl sulfate based on the total amount of bentonite, and stir thoroughly to obtain a bentonite conditioning liquid;

[0076] S104: Then put the product of S101 into 3 times of the bentonite conditioning liquid and ultrasonically disperse to obtain a coordination treatment liquid.

[0077] The power of ultrasonic dispersion of this embodiment is 350 W, and the ultrasonic time is 20 min.

[0078] The silane coupling agent of this embodiment is silane coupling agent KH560.

[0079] Embodiment 2.

[0080] The graphene-containing flame-retardant polyester fiber board of this embodiment comprises polyester fibers, modified graphene agent, flame retardant, and coordination treatment liquid, wherein the mass ratio of polyester fibers, modified graphene agent, flame retardant, and coordination treatment liquid is 11:5:0.5:15.

[0081] The preparation method of the flame-retardant polyester fiber board is as follows:

[0082] Step one: first put the polyester fibers into the coordination treatment liquid for primary stirring modification treatment;

[0083] Step two: preparation of the modified graphene agent;

[0084] Step three: then add the modified graphene agent and tributyl phosphate flame retardant to the product of step one for secondary stirring modification treatment;

[0085] Step four: then open the treatment and card into a web, cross-lay the web, and needle punch to reinforce, and then reinforce in a hot air oven at 180°C;

[0086] Step five: the product of step four is hot-pressed into graphene flame-retardant polyester fiber board at 0.7 MPa and 125℃.

[0087] Preparation of the modified graphene agent of the embodiment:

[0088] S01, graphene is added into hydrochloric acid solution at a weight ratio of 1:6, stirred uniformly, then 5% of lanthanum sulfate and 5% of alkyl sulfonate sodium of the total amount of graphene are added, stirred fully, then washed with water and dried;

[0089] S02, 10% of the ball milling modifier of the total amount of S01 product is added into the product of S01, ball milling modification is performed at a speed of 1250 r / min for 50 min, then washed with water and dried, to obtain the modified graphene agent.

[0090] The mass fraction of the hydrochloric acid solution of the embodiment is 6%.

[0091] The ball milling modifier of the embodiment includes the following raw materials by weight:

[0092] 6 parts of carboxymethyl cellulose, 15 parts of chitosan aqueous solution, 3 parts of phosphate buffer solution, 5 parts of hydroxyapatite and 0.5 parts of barium titanate.

[0093] The mass fraction of the chitosan aqueous solution of the embodiment is 10%, and the pH value of the phosphate buffer solution is 5.0.

[0094] The speed of the first-stage stirring modification treatment of the embodiment is 450 r / min, the stirring time is 40 min, and the stirring temperature is 45℃.

[0095] The speed of the first-stage stirring modification treatment of the embodiment is 1200 r / min, the stirring time is 20 min, and the stirring temperature is 48℃.

[0096] The preparation method of the coordination treatment liquid of the embodiment is as follows:

[0097] S101: the silicon carbide whisker is heat-treated at 150℃ for 10 min, then heated to 220℃ at a rate of 3℃ / min, kept for 20 min, and then decreased to 45℃ at a rate of 5℃ / min;

[0098] S102: the bentonite is put into 5 times of ethanol solvent, stirred and dispersed uniformly to obtain bentonite suspension; 4 parts of silane coupling agent, 3 parts of Tween 60 and 10 parts of tetra-n-propyl zirconate are added into 25 parts of the bentonite suspension, stirred fully, then washed with water and dried to obtain the bentonite coordination agent;

[0099] S103: The bentonite coordinator is stirred in 10 times deionized water, and then 5% sodium alginate and 5% sodium dodecyl sulfate are added to the total amount of bentonite, and stirred thoroughly to obtain the adjusted bentonite liquid;

[0100] S104: Then the product of S101 is placed in 5 times the adjusted bentonite liquid for ultrasonic dispersion to obtain the coordinated treatment liquid.

[0101] The power of ultrasonic dispersion in this embodiment is 400W, and the ultrasonic time is 30min.

[0102] The silane coupling agent in this embodiment is silane coupling agent KH560.

[0103] Example 3.

[0104] The graphene modified polyester fiber board in this embodiment includes polyester fiber, modified graphene agent, flame retardant, and coordinated treatment liquid, wherein the mass ratio of polyester fiber, modified graphene agent, flame retardant, and coordinated treatment liquid is 10:4:0.5:14.

[0105] The preparation method of the flame-retardant polyester fiber board is as follows:

[0106] Step one: First, the polyester fiber is sent into the coordinated treatment liquid for primary stirring and modification treatment.

[0107] Step two: Preparation of modified graphene agent

[0108] Step three: Then the modified graphene agent and tributyl phosphate flame retardant are added to the product of step one for secondary stirring and modification treatment.

[0109] Step four: Then, after opening and treating, it is carded into a web, cross-laid, and needle-punched for reinforcement, and then hot air reinforced in an oven at 180℃.

[0110] Step five: The product of step four is placed in a hot press at 0.6MPa and 125℃ to form a graphene modified polyester fiber board.

[0111] Preparation of the modified graphene agent in this embodiment:

[0112] S01: Graphene is added to the hydrochloric acid solution in a weight ratio of 1:6 and stirred uniformly, and then 3.5% lanthanum sulfate and 3% sodium alkyl sulfonate are added to the total amount of graphene, and stirred thoroughly, and then washed with water and dried.

[0113] S02: 7.5% ball milling modifier is added to the product of S01, and the ball milling modification is performed at a speed of 1200r / min for 45min, and then washed with water and dried to obtain the modified graphene agent.

[0114] The mass fraction of the hydrochloric acid solution of this embodiment is 4.5%.

[0115] The ball mill modifier of this embodiment includes the following raw materials by weight:

[0116] 4.5 parts of carboxymethyl cellulose, 12.5 parts of chitosan aqueous solution, 2 parts of phosphate buffer solution, 3.5 parts of hydroxyapatite, and 0.35 parts of barium titanate.

[0117] The mass fraction of the chitosan aqueous solution of this embodiment is 8%, and the pH value of the phosphate buffer solution is 5.0.

[0118] The rotation speed of the primary stirring modification treatment of this embodiment is 400 r / min, the stirring time is 35 min, and the stirring temperature is 42℃.

[0119] The rotation speed of the primary stirring modification treatment of this embodiment is 1000 r / min, the stirring time is 15 min, and the stirring temperature is 47℃.

[0120] The preparation method of the coordination treatment liquid of this embodiment is:

[0121] S101: heat-treating the silicon carbide whisker at 145℃ for 7.5 min, then increasing the temperature to 215℃ at a rate of 2℃ / min, keeping the temperature for 15 min, and then decreasing the temperature to 42℃ at a rate of 4℃ / min;

[0122] S102: sending the bentonite into 4 times of ethanol solvent, stirring and dispersing uniformly to obtain a bentonite suspension; adding 2.5 parts of silane coupling agent, 2 parts of Tween 60, and 7.5 parts of tetra-n-propyl zirconate into 20 parts of the bentonite suspension, stirring fully, and finally washing with water and drying to obtain a bentonite coordination agent;

[0123] S103: sending the bentonite coordination agent into 7.5 times of deionized water and stirring uniformly, then adding sodium alginate of 3.5% and sodium dodecyl sulfate of 3% of the total amount of bentonite, stirring fully, to obtain an adjusted bentonite liquid;

[0124] S104: then placing the product of S101 in 4 times of the adjusted bentonite liquid for ultrasonic dispersion to obtain a coordination treatment liquid.

[0125] The power of the ultrasonic dispersion of this embodiment is 380 W, and the ultrasonic time is 25 min.

[0126] The silane coupling agent of this embodiment is silane coupling agent KH560.

[0127] Comparative Example 1.

[0128] Different from Example 3 is that the coordination treatment liquid is not used.

[0129] Comparative Example 2.

[0130] The difference between Example 3 is that the S101 product is not added in the preparation of the coordination treatment liquid.

[0131] Comparative Example 3.

[0132] The difference between Example 3 is that bentonite is used instead of bentonite in the bentonite coordination agent.

[0133] Comparative Example 4.

[0134] The difference between Example 3 is that tetra-n-propyl zirconate is not added in the bentonite coordination agent.

[0135] Comparative Example 5.

[0136] The difference between Example 3 is that the modified graphene agent is not added.

[0137] Comparative Example 6.

[0138] The difference between Example 3 is that graphene is used instead of modified graphene agent in the preparation of the modified graphene agent.

[0139] Comparative Example 7.

[0140] The difference between Example 3 is that the modified graphene agent is not treated with a ball mill modifier in the preparation of the modified graphene agent.

[0141] Comparative Example 8.

[0142] The difference between Example 3 is that lanthanum sulfate is not added in the preparation of the modified graphene agent.

[0143] The products of Examples 1-3 and Comparative Examples 1-8 are tested for flame retardation and sound absorption performance. The thickness of the selected product is 20mm, and the performance test at 1000Hz is tested. At the same time, the product is tested under normal conditions, and after being soaked in 2% hydrochloric acid for 12h, it is taken out and tested for performance under acid corrosion conditions.

[0144]

[0145]

[0146] From Comparative Examples 1-8 and Examples 1-3, it can be seen that the product of Example 3 has excellent sound absorption and flame retardation, and both can significantly improve the coordination effect. At the same time, the product has excellent performance stability under acid corrosion conditions.

[0147] From Comparative Examples 1-4 and Example 3, it can be seen that the sound absorption and flame retardation of the product are significantly deteriorated without using the coordination treatment liquid. The performance of the product has a deteriorating trend without adding S101 product in the coordination treatment liquid, using bentonite instead of bentonite in the bentonite coordination agent, and not adding tetra-n-propyl zirconate in the bentonite coordination agent. Only the coordination treatment liquid prepared by the method of the present application has the most significant performance effect.

[0148] From the comparative example 5-8 and example 3, it can be seen that the sound absorption and the flame retardation of the product have a deteriorating trend without adding the modified graphene agent, the sound absorption and the flame retardation of the product have a synergistic effect with the coordination treatment liquid treatment, and the performance effect of the product is the most significant;

[0149] Meanwhile, the performance of the product is more obviously deteriorated under the acid corrosion condition with the modified graphene agent instead of the graphene, and the performance effect of the product has a deteriorating trend without using the ball milling modifier for the preparation of the modified graphene agent and without adding the lanthanum sulfate in the preparation of the modified graphene agent, and only the performance effect of the product is the most significant with the modified graphene agent prepared by the method of the application.

[0150] It is found from the above test that the ball milling modifier has a great effect on the performance of the product, and based on this, the application is further explored:

[0151] Experimental example 1

[0152] The raw materials of the product are the same as those of example 3, and the only difference is that the chitosan aqueous solution is not added.

[0153] Experimental example 2

[0154] The raw materials of the product are the same as those of example 3, and the only difference is that the hydroxyapatite is not added.

[0155] Experimental example 3

[0156] The raw materials of the product are the same as those of example 3, and the only difference is that the barium titanate is not added.

[0157] Experimental example 4

[0158] The raw materials of the product are the same as those of example 3, and the only difference is that the carboxymethyl cellulose is not added.

[0159] Experimental example 5

[0160] The raw materials of the product are the same as those of example 3, and the only difference is that the mass fraction of the chitosan aqueous solution is 12%.

[0161]

[0162] It can be seen from experimental examples 1-5 that the performance of the product is obviously deteriorated without adding the hydroxyapatite in the ball milling modifier, which shows that the hydroxyapatite has an important influence on the performance of the product in the ball milling modifier, and the performance of the product has a deteriorating trend without adding the barium titanate and the chitosan aqueous solution, and the performance effect of the product is the best with the ball milling modifier prepared by the hydroxyapatite, the barium titanate, the chitosan aqueous solution and the carboxymethyl cellulose, and thus the performance effect of the product is the most significant with the ball milling modifier of the application.

[0163] It will be obvious to a person skilled in the art that the application is not limited to the details of the above-described exemplary embodiments, but that the application can be implemented in other embodiments without departing from the scope of the application. The embodiments are therefore to be seen as exemplary and in no way restrictive, the scope of the application being defined by the claims below rather than by the above description, and all variations falling within the meaning and range of equivalency of the essential characteristics of the claims are therefore intended to be embraced therein.

[0164] Furthermore, it should be understood that although the description is made according to embodiments, not every embodiment contains only one independent technical solution, and the description is made in this way only for the sake of clarity, and a person skilled in the art should consider the description as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by a person skilled in the art.

Claims

1. A graphene-based flame-retardant polyester fiber board, characterized in that, The fiberboard includes polyester fiber, modified graphene agent, flame retardant, and blending treatment liquid, wherein the mass ratio of polyester fiber, modified graphene agent, flame retardant, and blending treatment liquid is (9-11):(3-5):0.5:(13-15). The preparation method of flame-retardant polyester fiber board is as follows: Step 1: First, the polyester fiber is fed into the coordinating treatment solution for primary stirring and modification treatment; Step 2: Preparation of modified graphene agent; Step 3: Then, the modified graphene agent and tributyl phosphate flame retardant are added to the product of Step 1 for secondary stirring modification treatment; Step 4: After further loosening, the wire is combed into a web, cross-laid, needle-punched for reinforcement, and then reinforced with hot air in a 180℃ oven. Step 5: The product from Step 4 is hot-pressed at 0.5-0.7 MPa and 125℃ to prepare graphene flame-retardant polyester fiber board. Preparation of the modified graphene agent: S01, add graphene to hydrochloric acid solution at a weight ratio of 1:6 and stir until uniform. Then add 2-5% of lanthanum sulfate and 1-5% of sodium alkyl sulfonate of the total amount of graphene, stir thoroughly, and then wash with water and dry. SO2, add 5-10% of the total amount of SO1 product to the SO1 product and ball milling modification. The ball milling speed is 1150-1250 r / min and the ball milling time is 40-50 min. After ball milling, wash with water and dry to obtain the modified graphene agent. The preparation method of the coordinated treatment liquid is as follows: S101: Heat-treat silicon carbide whiskers at 140-150℃ for 5-10 min, then raise the temperature to 210-220℃ at a rate of 1-3℃ / min, hold for 10-20 min, and then lower the temperature to 40-45℃ at a rate of 3-5℃ / min. S102: Add bentonite to 3-5 times its volume of ethanol solvent, stir and disperse evenly to obtain a bentonite suspension; Add 1-4 parts of silane coupling agent, 1-3 parts of Tween 60 and 5-10 parts of tetra-n-propylzirconate to 15-25 parts of bentonite suspension, stir thoroughly, and finally wash with water and dry to obtain bentonite synergist. S103: Add the bentonite conditioner to 5-10 times the amount of deionized water and stir evenly. Then add 2-5% sodium alginate and 1-5% sodium dodecyl sulfate of the total bentonite amount and stir thoroughly to obtain the bentonite conditioning solution. S104: Then the S101 product is placed in 3-5 times the volume of adjusted bentonite solution and ultrasonically dispersed to obtain the coordinated treatment solution.

2. The graphene flame-retardant polyester fiber board according to claim 1, characterized in that, The hydrochloric acid solution has a mass fraction of 3-6%.

3. The graphene flame-retardant polyester fiber board according to claim 1, characterized in that, The ball milling modifier comprises the following raw materials in parts by weight: 3-6 parts carboxymethyl cellulose, 10-15 parts chitosan aqueous solution, 1-3 parts phosphate buffer solution, 2-5 parts hydroxyapatite and 0.2-0.5 parts barium titanate.

4. The graphene flame-retardant polyester fiber board according to claim 3, characterized in that, The chitosan aqueous solution has a mass fraction of 6-10%; the phosphate buffer solution has a pH of 5.

0.

5. The graphene flame-retardant polyester fiber board according to claim 1, characterized in that, The stirring speed for the first-stage stirring modification treatment is 350-450 r / min, the stirring time is 30-40 min, and the stirring temperature is 40-45℃.

6. The graphene flame-retardant polyester fiber board according to claim 1, characterized in that, The primary stirring modification treatment involves a stirring speed of 800-1200 r / min, a stirring time of 10-20 min, and a stirring temperature of 46-48℃.

7. The graphene flame-retardant polyester fiber board according to claim 1, characterized in that, The ultrasonic dispersion power is 350-400W, and the ultrasonic time is 20-30min.

8. The graphene flame-retardant polyester fiber board according to claim 1, characterized in that, The silane coupling agent is silane coupling agent KH560.

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