Organosilicon flame-retardant material as well as preparation method and application thereof

Abstract

The invention discloses an organic silicon flame-retardant material and a preparation method and application thereof, and the preparation method comprises the following preparation steps: S1, hexamethylenediamine and soybean flavone diglycidyl ether are subjected to a reaction to prepare a first intermediate; s2, ethanol amine and epoxidized soybean oil are subjected to a reaction, and a second intermediate is prepared; s3, reacting side-chain epoxy silicone oil, the first intermediate, the second intermediate and a curing agent in a solvent, and then adding an initiator to prepare the organic silicon flame-retardant material. According to the organic silicon flame-retardant material finishing agent provided by the invention, a fabric can be endowed with relatively good flame-retardant effect and soft skin-friendly effect at the same time through one-step finishing, the problem that two finishing agents, namely a flame-retardant finishing agent and a skin-friendly finishing agent, are used for resisting against each other is avoided, the finishing process of the fabric is simplified, and the finishing efficiency is improved.

Description

Technical Field

[0001] The present application relates to the field of polymer materials, and in particular to an organic silicon flame retardant material, a preparation method and applications thereof. Background Art

[0002] In the modern textile industry, functional demands on clothing are becoming increasingly diverse, and flame retardancy has become a key indicator for improving clothing safety. As people's living and working environments change, the requirements for clothing fire resistance and flame retardancy are becoming increasingly stringent. Whether working in industrial production environments where people may be exposed to open flames and high temperatures, or coping with potential fire risks in daily life, flame-retardant clothing can provide a more reliable safety guarantee.

[0003] However, traditional silicone finishes have significant shortcomings in terms of flame retardancy. Conventional silicone finishes such as hydroxyl silicone oils, amino silicone oils, and polyether-modified silicone oils, while offering excellent softness and hand feel, are unable to impart good flame retardancy to clothing. In the event of a fire, these finishes are unable to effectively prevent the clothing from burning, making it difficult to ensure the safety of the wearer. Furthermore, these finishes have a weak bond with clothing fibers and are easily washed off the surface of clothing during daily washing. With increasing frequency of washing, the effectiveness of the finish gradually decreases, and the clothing's flexibility, wrinkle resistance, and other properties also decline, making it impossible to maintain good long-term performance.

[0004] To improve the flame retardancy of clothing, existing technologies often employ the addition of flame retardants. However, their application in clothing finishes presents numerous challenges. For one thing, common flame retardants lack compatibility with silicone finishes. When mixed, the flame retardants are difficult to evenly disperse within the silicone finish system, and agglomeration is likely to occur. This not only impacts the stability of the finish, but also prevents the flame retardant from evenly adhering to the surface of the fabric during finishing. This results in uneven flame retardancy and poor flame retardancy in some areas. Furthermore, the addition of some flame retardants can negatively impact other properties of clothing, such as its feel and color. For example, the addition of some inorganic flame retardants can make clothing feel harder, affecting wearer comfort. Certain flame retardants can also chemically react with dyes in clothing, altering its color and reducing its aesthetic appeal.

[0005] Furthermore, the durability of existing silicone flame-retardant finishes is insufficient in the face of frequent washing. After repeated washing, the flame-retardant components in the finish are easily lost, significantly reducing the flame-retardant properties of the garment. For specialized workwear requiring long-term flame retardancy, such as firefighter uniforms and powerwork uniforms, this durability issue severely impacts the garment's practical value and safety. Summary of the Invention

[0006] The purpose of the present application is to provide an organic silicon flame retardant material which, after being applied to a fabric finishing agent, imparts flame retardancy to the fabric while maintaining its softness.

[0007] To achieve the above objectives, the technical solution adopted in this application is to provide an organic silicon flame retardant material with the general structural formula: , Where M1 is ; M2 is ; R is ; R1 is ; M3 is .

[0008] n, a, b, c, d, x, y, z are integers, and 73≤n≤137; 2≤a≤3; 3≤b≤4; 3≤c≤4; 3≤d≤4, 3≤x+z≤6; 9≤y≤20.

[0009] The present application also provides a method for preparing an organic silicon flame retardant material, comprising the following preparation steps: S1: Hexamethylenediamine reacts with daidzein diglycidyl ether to prepare a first intermediate; S2: Ethanolamine reacts with epoxidized soybean oil to produce the second intermediate; S3: reacting the side chain epoxy silicone oil, the first intermediate, the second intermediate and a curing agent in a solvent, and then adding an initiator to prepare an organosilicon flame retardant material; The general structural formula of the first intermediate is: ; The general structural formula of the second intermediate is: , where R is ; R1 is ; The general structural formula of the organosilicon flame retardant material is: , Where M1 is ; M2 is ; R is ; R1 is ; M3 is .

[0010] n, a, b, c, d, x, y, z are integers, and 73≤n≤137; 2≤a≤3; 3≤b≤4; 3≤c≤4; 3≤d≤4, 3≤x+z≤6; 9≤y≤20.

[0011] As a preference, the number average molecular weight of the side chain epoxy silicone oil is 8000-10000.

[0012] As another preference, the number of epoxy groups in the side chain epoxy silicone oil is k, and 11≤k≤15.

[0013] As another preference, the curing agent is polyetheramine, and the polyetheramine is any one of Huntsman ED600, ED900 and ED1200.

[0014] As another preference, the solvent is one of isopropyl alcohol, ethylene glycol monobutyl ether, and diethylene glycol monobutyl ether.

[0015] As another preferred embodiment, the step S1 is specifically as follows: adding 300-400 parts of a hexamethylenediamine aqueous solution and 100-200 parts of isopropanol to a reaction vessel, heating the reaction vessel to 45-55° C., slowly adding 300-400 parts of soybean flavonoid diglycidyl ether dropwise to the reaction vessel, and after the addition is complete, heating the reaction vessel to 60-70° C. and keeping the temperature for 3-5 hours to obtain the first intermediate.

[0016] As another preferred embodiment, the S2 step is specifically as follows: adding 100-200 parts of the ethanolamine and 400-600 parts of isopropanol to a reaction vessel, stirring thoroughly, heating to 45-55° C., slowly adding 800-900 parts of the epoxidized soybean oil dropwise to the reaction vessel, heating to 65-75° C. after the addition is completed, and keeping warm for 4-6 hours to obtain the second intermediate.

[0017] Further preferably, the S3 step is specifically as follows: adding 800-1000 parts of the side chain epoxy silicone oil, 240-320 parts of the first intermediate, 464-618 parts of the second intermediate, 180-480 parts of the polyether amine and 1250-1840 parts of the solvent to a reaction vessel, stirring thoroughly, heating to 75-90°C, keeping warm for 8-15 hours, adding 15-20 parts of glacial acetic acid, and preparing the silicone flame retardant material.

[0018] The present application also provides an organosilicon flame retardant material finishing agent, which includes the following preparation raw materials: an emulsifier, a solvent, and the above-mentioned organosilicon flame retardant material.

[0019] Compared with the prior art, the present invention has the following advantages: (1) This application utilizes the synergistic effect of epoxy soybean oil, soybean flavone diglycidyl ether and polysiloxane to give the product excellent flame retardant effect without affecting the comfort of the fabric; (2) The organic silicone flame retardant finishing agent provided in this application can give the fabric a good flame retardant effect and a soft skin-friendly effect in one step, avoiding the conflict between the flame retardant finishing agent and the skin-friendly finishing agent when used separately, simplifying the fabric finishing process and improving the finishing efficiency. DETAILED DESCRIPTION

[0020] Below, the present application is further described in conjunction with specific implementation methods. It should be noted that, under the premise of no conflict, the various embodiments or technical features described below can be arbitrarily combined to form new embodiments.

[0021] The terms "comprises" and "having" and any variations thereof in the specification and claims of this application are intended to cover non-exclusive inclusions. For example, a process, method, system, product or apparatus that includes a series of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, product or apparatus.

[0022] The present application provides an organic silicon flame retardant material, the general structure of which is as follows: , Where M1 is ; M2 is ; R is ; R1 is ; M3 is .

[0023] n, a, b, c, d, x, y, z are integers, and 73≤n≤137; 2≤a≤3; 3≤b≤4; 3≤c≤4; 3≤d≤4, 3≤x+z≤6; 9≤y≤20.

[0024] The organosilicon flame retardant material provided in this application introduces a large number of epoxy groups and amino groups into the product structure. These groups can self-crosslink during the high-temperature setting process to form a dense film on the surface of the textile, so that the heat transfer of the treated fabric is interrupted during the combustion process, and the system temperature is lower than the ignition point of the combustion, thereby causing self-extinguishing behavior.

[0025] The organic silicon flame retardant material of the present application does not introduce flame retardant elements such as halogen and phosphorus contained in traditional flame retardants, thus avoiding harm to human body and environment and meeting the requirements of green and environmental protection development.

[0026] The silicone flame retardant material of the present application introduces polysiloxane and amino groups into the product structure. While improving the softness and hand comfort of the fabric through the silicone group, it further reduces the negative impact of the resin material on the comfort of the fabric, ensuring that the treated fabric has better wearing comfort.

[0027] The present application also provides a method for preparing an organic silicon flame retardant material, comprising the following steps: S1: Hexamethylenediamine reacts with daidzein diglycidyl ether to prepare a first intermediate; S2: Ethanolamine reacts with epoxidized soybean oil to produce the second intermediate; S3: reacting the side chain epoxy silicone oil, the first intermediate, the second intermediate and the curing agent in a solvent, and then adding an initiator to prepare the organic silicone flame retardant material of the present application.

[0028] The general structural formula of the first intermediate is:

[0029] The reaction formula of the reaction between hexamethylenediamine and soybean flavonoid diglycidyl ether is:

[0030] In some embodiments, step S1 is specifically as follows: adding a hexamethylenediamine aqueous solution and a solvent to a reaction vessel, heating the temperature to 45-55°C, slowly adding soybean flavonoid diglycidyl ether dropwise to the reaction vessel, and after the addition is completed, heating the temperature to 65-90°C and keeping the temperature for 3-7 hours to obtain a first intermediate.

[0031] The general structural formula of the second intermediate is: , where R is ; R1 is .

[0032] The reaction formula of ethanolamine and epoxidized soybean oil is as follows: , where R is ; R1 is .

[0033] In some embodiments, step S2 is specifically as follows: adding ethanolamine and the corresponding solvent to a reaction vessel, heating the temperature to 45-55°C, slowly adding epoxy soybean oil dropwise to the reaction vessel, heating the temperature to 65-75°C after the addition is completed, and keeping the temperature for 4-6 hours to obtain a second intermediate.

[0034] The reaction formula of the side chain epoxy silicone oil, the first intermediate, the second intermediate and the curing agent is: , where M1 is ; M2 is ; R is ; R1 is ; M3 is ; m, n, a, b, c, d, x, y, z are integers, and 11≤m≤15; 73≤n≤137; 2≤a≤3; 3≤b≤4; 3≤c≤4; 3≤d≤4, 3≤x+z≤6; 9≤y≤20.

[0035] In some embodiments, the number average molecular weight of the side chain epoxy silicone oil is 8000 to 10000. The higher the number average molecular weight, the longer the silicone oil molecular chain, the stronger the intermolecular force, resulting in a significant increase in the viscosity of the system, and a thicker and more flexible film.

[0036] In some embodiments, the number of epoxy groups in the side-chain epoxy silicone oil is k, where 11 ≤ k ≤ 15. The number of epoxy groups in the side-chain epoxy silicone oil is a key factor in determining the reaction process, product structure, and application performance. Epoxy groups serve as crosslinking points, and their number directly determines the crosslink density of the final finishing agent.

[0037] In some embodiments, the curing agent is a polyetheramine, preferably any one of Huntsman ED600, ED900, and ED1200. The choice of polyetheramine has little effect on the flame retardancy of the final silicone flame retardant material, but has a relatively large impact on the softness and comfort of the fabric.

[0038] In some embodiments, the initiator is glacial acetic acid.

[0039] In some embodiments, the reaction time in step S3 is 6 to 16 hours. Prolonging the reaction time in step S3 is beneficial to improving the flame retardant effect, but too long a reaction time will reduce the softness and comfort of the fabric.

[0040] In some embodiments, the solvent in step S3 is any one of isopropyl alcohol, ethylene glycol monobutyl ether, or diethylene glycol monobutyl ether. The solvent has little effect on the flame retardancy and comfort of the organosilicon finishing agent material.

[0041] In some embodiments, the specific preparation method of the organosilicon flame retardant material is as follows, calculated by weight: S1: adding 300-400 parts of a hexamethylenediamine aqueous solution and 100-200 parts of isopropyl alcohol to a reaction vessel, heating the temperature to 45-55°C, slowly adding 300-400 parts of soybean flavonoid diglycidyl ether dropwise to the reaction vessel, heating the temperature to 60-70°C after the addition is complete, and keeping the temperature for 3-5 hours to obtain a first intermediate, wherein the concentration of the hexamethylenediamine aqueous solution is 65-75%; S2: Add 100-200 parts of ethanolamine and 400-600 parts of isopropanol to a reaction vessel, stir thoroughly, raise the temperature to 45-55°C, slowly dropwise add 800-900 parts of epoxidized soybean oil to the reaction vessel, raise the temperature to 65-75°C after the addition is complete, and keep the temperature for 4-6 hours to obtain a second intermediate; S3: Add 800-1000 parts of side chain epoxy silicone oil, 240-320 parts of the first intermediate, 464-618 parts of the second intermediate, 180-480 parts of polyetheramine and 1250-1840 parts of solvent to the reactor, stir thoroughly, heat to 75-90°C, keep warm for 8-15 hours, add 15-20 parts of glacial acetic acid to prepare the silicone flame retardant finishing agent of the present application.

[0042] This application primarily utilizes an epoxy curing mechanism to introduce amino groups into soybean brass diglycidyl ether and epoxy soybean oil. This amino group then undergoes a curing reaction with epoxy silicone oil to produce a flame-retardant organosilicon material. This organosilicon flame-retardant material achieves flame retardancy by interrupting heat exchange. During the high-temperature setting process, a dense film primarily composed of polysiloxane, soybean flavone diglycidyl ether, and epoxy soybean oil forms on the fabric surface. This film, which has low inherent flammability, interrupts heat transfer during fabric combustion, causing the fabric temperature to fall below its ignition point, leading to self-extinguishing.

[0043] The present application utilizes the synergistic effect of epoxy soybean oil, soybean flavonoid diglycidyl ether and polysiloxane to give the product an excellent flame retardant effect without affecting the comfort of the fabric.

[0044] The organic silicon flame retardant material provided in this application has good carbon-forming ability under the action of curing agent in the soybean flavone diglycidyl ether and epoxy soybean oil introduced into the product structure. The complete and dense carbon layer formed after combustion combines with the organic silicon and has excellent flame retardant properties.

[0045] The present application provides an organosilicon flame retardant material finishing agent, comprising the above-mentioned organosilicon flame retardant material, an emulsifier, a solvent and glacial acetic acid.

[0046] The present application provides a method for preparing an organosilicon flame retardant material finishing agent, comprising the following preparation steps, calculated by mass: emulsifying 80-120 parts of the above-mentioned organosilicon flame retardant material, 200-240 parts of water, 5-15 parts of emulsifier and 1-4 parts of glacial acetic acid to obtain an organosilicon flame retardant material finishing agent of the present application.

[0047] The organic silicon flame retardant material finishing agent provided in the present application can simultaneously give the fabric good flame retardant effect and soft skin-friendly effect in one step, avoiding the conflict problem of using flame retardant finishing agent and skin-friendly finishing agent separately, simplifying the fabric finishing process and improving finishing efficiency.

[0048] Example 1 Preparation of an organic silicon flame retardant material, comprising the following preparation steps, calculated by weight: S1: 331 parts of a 70% by mass aqueous solution of hexamethylenediamine and 133 parts of isopropyl alcohol were added to a reaction kettle, and the temperature was raised to 55°C. 366 parts of soybean flavonoid diglycidyl ether were slowly added dropwise to the reaction kettle. After the addition was complete, the temperature was raised to 70°C and kept at this temperature for 5 hours to obtain a first intermediate. S2: 183 parts of ethanolamine and 500 parts of isopropanol were added to a reactor, stirred thoroughly, and heated to 55°C. 863 parts of epoxidized soybean oil were slowly added dropwise to the reactor. After the addition was completed, the temperature was raised to 75°C and kept at this temperature for 6 hours to obtain a second intermediate. S3: 800 parts of side chain epoxy silicone oil with a number average molecular weight of 8000, 240 parts of the first intermediate, 464 parts of the second intermediate, 180 parts of polyetheramine Huntsman ED600 and 1250 parts of isopropyl alcohol are added to the reactor, the number of epoxy groups contained in the side chain epoxy silicone oil is 15, the raw materials are fully stirred, the temperature is raised to 75°C, and the temperature is kept for 8 hours. 15 parts of glacial acetic acid are added to obtain the silicone flame retardant material of the present application.

[0049] Example 2 The holding time in step S3 was adjusted to 15 hours, and the other preparation steps were consistent with those in Example 1.

[0050] Example 3 The polyetheramine in step S3 was replaced with 270 parts by mass of polyetheramine Huntsman ED900, and the other preparation steps were consistent with those of Example 1.

[0051] Example 4 The polyetheramine in step S3 was replaced with 360 parts by mass of polyetheramine Huntsman ED1200, and the other preparation steps were consistent with those of Example 1.

[0052] Example 5 The solvent in step S3 was adjusted to 1250 parts by mass of ethylene glycol monobutyl ether, and the other preparation steps were consistent with those in Example 2.

[0053] Example 6 The solvent in step S3 was adjusted to 1250 parts by mass of diethylene glycol monobutyl ether, and the other preparation steps were consistent with those in Example 2.

[0054] Example 7 The amount of the first intermediate added in step S3 was adjusted to 332 parts by mass, and the other preparation steps were consistent with those in Example 2.

[0055] Example 8 The amount of the second intermediate added in step S3 was adjusted to 618 parts by mass, and the other preparation steps were consistent with those of Example 2.

[0056] Example 9 The amount of polyetheramine added in step S3 was adjusted to 240 parts by mass, and the other preparation steps were consistent with those in Example 2.

[0057] Example 10 The number average molecular weight of the side chain epoxy silicone oil in step S3 was adjusted to 11,000, and the other preparation steps were consistent with those in Example 2.

[0058] Example 11 The amount of the first intermediate in step S3 was adjusted to 332 parts by mass, and the amount of the second intermediate was adjusted to 618 parts by mass. The other preparation steps were consistent with those of Example 10.

[0059] Example 12 The amount of polyetheramine in step S3 was adjusted to 240 parts by mass, and the other preparation steps were consistent with those of Example 11.

[0060] Example 13 The number of epoxy groups in the side chain epoxy silicone oil in step S3 was adjusted to 11, and the other preparation steps were consistent with the preparation steps of Example 12.

[0061] Comparative Example 1 The soybean brass diglycidyl ether in step S1 was replaced with polyethylene glycol diglycidyl ether with a number average molecular weight of 400, and the other preparation steps were consistent with those of Example 12.

[0062] Comparative Example 2 The epoxy soybean oil in step S2 was replaced with glyceryl propoxy triglycidyl ether, and the other preparation steps were consistent with those of Example 12.

[0063] Comparative Example 3 Purchase commercially available organophosphorus flame retardant finishing agents.

[0064] Comparative Example 4 Purchase commercially available inorganic phosphorus-nitrogen flame retardant finishing agents.

[0065] The flame retardant materials of the above embodiments and comparative examples were emulsified and the fabrics were treated according to the following steps: Emulsification step: 100 parts by mass of the flame retardant finishing agent of the above embodiments or comparative examples, 220 parts by mass of water, 10 parts by mass of emulsifier 1350 and 2 parts by mass of glacial acetic acid are emulsified in a homogenizer to obtain the silicone flame retardant finishing agent of the present application.

[0066] Finishing steps: Cotton fabric and polyester fabric are respectively dipped into the working liquid, the working liquid is 70~80g / L of the emulsion of the product of this application, soaked for 20 minutes, double dipped and double rolled, and then baked in an oven with the temperature set at 180~190℃ and the baking time set at 2~3min. After regaining moisture for 1 hour, the fabric performance evaluation test is performed.

[0067] Performance evaluation test 1. Hand feel evaluation test: Use the hand touch method to evaluate the comprehensive hand feel, using a 0-5 point evaluation method, with 0 being the worst and 5 being the best. 10 people evaluate at the same time and take the average value.

[0068] 2. Softness Test: According to GB / T 18318 "Textiles - Determination of Fabric Bending Length": Place a long strip of test specimen on a platform. Press a ruler against the specimen, with the specimen's long axis parallel to the ruler's length. Move the ruler and the specimen's long axis simultaneously on the platform, allowing the portion of the specimen protruding from the platform to hang suspended in the air. Bend under its own weight. When the downwardly bent end of the specimen touches a surface inclined at a 41.5° angle to the horizontal, half the extended length of the specimen is considered the bending length. The specimen's flexural stiffness is calculated from the bending length and the mass per unit area.

[0069] Sample: 6 pieces of 25mm*25mm warp and weft knitted fabrics, each piece is measured 4 times and the average value is taken; Calculation of bending stiffness: G=mC 3 10 -2 Where: G is the bending stiffness per unit width, mN·cm; m——mass per unit area of ​​sample, g / m 2 ; C——average bending length of the specimen, cm 3. Vertical burning test: According to GB / T5455-2014 "Textile combustion performance - Determination of vertical direction damage length, smoldering and afterflaming time", each sample is measured 5 times and the average value is taken.

[0070] 4. Limiting oxygen index test: Tested according to GB / T5454-1997 "Textile combustion performance test oxygen index method".

[0071] The performance of cotton fabrics treated with the organic silicon flame retardant finishing agents prepared in each example and the flame retardant finishing agent of the comparative example was tested, and the performance test results are recorded in Table 1 below.

[0072] Table 1 Test results of the flame retardant products of various embodiments and comparative examples on cotton fabrics

[0073] Analysis of the performance test results of Comparative Example 1, Comparative Example 2 and Example 12 in Table 1 shows that the present application uses soy flavonoid diglycidyl ether and epoxy soybean oil as raw materials to prepare silicone flame retardant materials, which can make cotton fabrics have better flame retardant effects and effectively reduce the damaged length of cotton fabrics.

[0074] Analysis of the performance test results of Comparative Examples 3, 4, and Example 12 shows that the organosilicon flame retardant finish product of the present application can achieve a flame retardant effect similar to that of commercially available organophosphorus flame retardant finishes and inorganic phosphorus-nitrogen flame retardant finishes. However, the commercially available flame retardant finishes reduced the hand feel of cotton fabric after finishing, with a flexural stiffness exceeding 40 mN.cm, resulting in a stiff feel and receiving the worst hand evaluation.

[0075] The performance of polyester fabrics treated with the organic silicon flame retardant finishing agents prepared in each example and the flame retardant finishing agent of the comparative example was tested, and the performance test results are recorded in Table 2 below.

[0076] Table 2 Performance test results of flame retardant products of various embodiments and comparative examples on polyester fabrics

[0077] Analysis of the performance test results in Table 2 shows that the silicone flame retardant finishing agent of the present application also exhibits a good treatment effect on polyester fabrics. While imparting a good flame retardant effect to polyester fabrics, it also improves the softness and feel of the fabric, allowing the fabric to maintain comfort while improving functionality.

[0078] Compared with commercially available organophosphorus flame retardant finishing agents and inorganic phosphorus nitrogen flame retardant finishing agents, the organosilicon flame retardant finishing agent of the present application exhibits an effect similar to that of cotton fabric on polyester fabric, and the flame retardant effect is close to that of commercially available flame retardant finishing agents, but the softness and comfort are far superior to those of commercially available flame retardant finishing agents, and the overall effect is better than that of commercially available flame retardant finishing agents.

[0079] Analysis of the performance test results of Examples 1 and 2 in Tables 1 and 2 shows that extending the reaction time in step S3 can increase the degree of reaction crosslinking to a certain extent, thereby improving the flame retardant effect of the silicone flame retardant, but the feel and softness of the fabric are slightly reduced.

[0080] Analysis of the performance test results of Examples 2, 3, and 4 in Tables 1 and 2 shows that the selection of different polyetheramines in step S3 has little effect on the flame retardancy of the fabric, but exhibits differences in comfort. The polyetheramine Huntsman ED600 is preferred, as it achieves better overall performance.

[0081] Analysis of the performance test results of Examples 2, 5, and 6 in Tables 1 and 2 shows that selecting isopropyl alcohol, ethylene glycol monobutyl ether, and diethylene glycol monobutyl ether as solvents in step S3, respectively, has little effect on the flame retardancy and comfort of the resulting silicone finishing agent.

[0082] By analyzing the performance test results of Examples 9 to 12 in Tables 1 and 2, adjusting the first intermediate and the second intermediate in step S3, that is, indirectly adjusting the addition amounts of soy flavonoid diglycidyl ether and epoxy soybean oil, has a certain impact on the flame retardant properties of the final silicone flame retardant finishing agent product, which indirectly illustrates the mechanism by which epoxy soybean oil and soy flavonoid diglycidyl ether impart excellent flame retardant properties to silicone flame retardant materials.

[0083] Compared with Example 12, changing the number of epoxy groups in the side chain epoxy silicone oil (K) slightly reduces the flame retardant effect, but still maintains a good effect. This is mainly due to the reduction of epoxy groups, which causes a slight decrease in the degree of high-stable crosslinking.

[0084] In summary, the organosilicon flame retardant finishing agent prepared in the present application is suitable for treating cotton fabrics and polyester fabrics, giving the fabrics excellent flame retardant effect and softness. While the fabrics have flame retardant function, they do not affect the consumer's wearing experience.

[0085] The above describes the basic principles, main features, and advantages of the present application. Those skilled in the art should understand that the present application is not limited to the above-described embodiments. The above-described embodiments and the specification merely illustrate the principles of the present application. Various changes and improvements may be made to the present application without departing from the spirit and scope of the present application. These changes and improvements fall within the scope of the present application for which protection is sought. The scope of protection claimed by the present application is defined by the appended claims and their equivalents.

Claims

1. An organic silicon flame retardant material, characterized in that: The general structural formula is: ， Where M1 is ; M2 is ; R is ; R1 is ; M3 is ; n, a, b, c, d, x, y, z are integers, and 73≤n≤137; 2≤a≤3; 3≤b≤4; 3≤c≤4; 3≤d≤4, 3≤x+z≤6; 9≤y≤20.

2. A method for preparing an organosilicon flame retardant material, characterized in that: The method comprises the following preparation steps: S1: Hexamethylenediamine reacts with daidzein diglycidyl ether to prepare a first intermediate; S2: Ethanolamine reacts with epoxidized soybean oil to produce the second intermediate; S3: reacting the side chain epoxy silicone oil, the first intermediate, the second intermediate and a curing agent in a solvent, and then adding an initiator to prepare an organosilicon flame retardant material; The general structural formula of the first intermediate is: ； The general structural formula of the second intermediate is: , where R is ; R1 is ; The general structural formula of the organosilicon flame retardant material is: ， Where M1 is ; M2 is ; R is ; R1 is ; M3 is ; n, a, b, c, d, x, y, z are integers, and 73≤n≤137; 2≤a≤3; 3≤b≤4; 3≤c≤4; 3≤d≤4, 3≤x+z≤6; 9≤y≤20.

3. The method for preparing an organosilicon flame retardant material according to claim 2, wherein: The number average molecular weight of the side chain epoxy silicone oil is 8000-10000.

4. The method for preparing an organosilicon flame retardant material according to claim 2, wherein: The number of epoxy groups in the side chain epoxy silicone oil is k, and 11≤k≤15.

5. The method for preparing the organic silicon flame retardant material according to claim 2, wherein: The curing agent is polyetheramine, and the polyetheramine is any one of Huntsman ED600, ED900 and ED1200.

6. The method for preparing the organic silicon flame retardant material according to claim X, wherein: The solvent is one of isopropyl alcohol, ethylene glycol monobutyl ether and diethylene glycol monobutyl ether.

7. The method for preparing an organosilicon flame retardant material according to claim 2, wherein: The step S1 specifically comprises: adding 300-400 parts of a hexamethylenediamine aqueous solution and 100-200 parts of isopropyl alcohol into a reaction container, heating the reaction container to 45-55° C., slowly dropwise adding 300-400 parts of soybean flavonoid diglycidyl ether into the reaction container, and after the dropwise addition is completed, heating the reaction container to 60-70° C. and keeping the temperature for 3-5 hours to obtain the first intermediate.

8. The method for preparing an organosilicon flame retardant material according to claim 2, wherein: The S2 step is specifically as follows: 100-200 parts of the ethanolamine and 400-600 parts of isopropanol are added to a reaction vessel, stirred thoroughly, and heated to 45-55° C., 800-900 parts of the epoxidized soybean oil are slowly added dropwise to the reaction vessel, and after the addition is completed, the temperature is raised to 65-75° C. and kept warm for 4-6 hours to obtain the second intermediate.

9. The method for preparing an organosilicon flame retardant material according to claim 5, wherein: The S3 step is specifically as follows: 800-1000 parts of the side chain epoxy silicone oil, 240-320 parts of the first intermediate, 464-618 parts of the second intermediate, 180-480 parts of the polyetheramine and 1250-1840 parts of the solvent are added to a reaction container, fully stirred, heated to 75-90° C., kept warm for 8-15 hours, and 15-20 parts of glacial acetic acid are added to obtain the silicone flame retardant material.

10. A finishing agent for organosilicon flame retardant material, characterized in that: The preparation method comprises the following raw materials: an emulsifier, a solvent, the organic silicon flame retardant material according to claim 1, or the organic silicon flame retardant material prepared by the preparation method according to claims 2 to 9.

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