Flame-retardant organic silicon light diffusant and preparation process thereof

By introducing boric acid and ammonium tripolyphosphate on the surface of the silicone light diffuser, combined with emulsification technology and surface modification treatment, the problem of insufficient flame retardant performance of existing light diffusers is solved, and the high temperature stability and transparency are improved. For the application of long, thin, soft and wide LED lights.

CN119119485APending Publication Date: 2024-12-13QUZHOU ZHONGTONG CHEM
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Patent Information

Application Number
CN202411471052.7
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-10-21
Publication Date
2024-12-13

AI Technical Summary

Technical Problem

The flame retardant properties of existing light diffusers are insufficient, making it difficult to meet the high-temperature welding process requirements of long, thin, soft and wide LED lamps, and at the same time affect the transparency and stability of the material.

Method used

By post-condensing the silicone core by hydrolysis of silicone, boric acid and ammonium tripolyphosphate are introduced on its surface, and micron-scale silicone light diffuser with flame retardant function is prepared.

Benefits of technology

It improves the flame retardant and chemical stability of silicone light diffuser, enhances its performance at high temperatures, ensures the transparency and stability of the material, and is suitable for long, thin, soft and wide LED lamp applications.

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Abstract

The invention relates to the technical field of organosilicone, and discloses a flame-retardant micron-sized organosilicone light diffusant and a preparation process thereof.The diffusant is composed of organosilicone and a flame retardant, surface modification is conducted on an organosilicone core through boric acid and ammonium tripolyphosphate, and the defect that the flame retardance of organosilicone is insufficient is overcome; the selected methyl silane has good chemical stability, low reactivity with other components, a flame-retardant effect and light diffusion performance, the pH value of a system is adjusted to be 3-4, an acid environment for silane hydrolysis is provided, the pH value of a condensation polymerization reaction is 8-10, and therefore the flame retardance of the material is improved; the boride and the phosphide modify the surfaces of the organic silicon microspheres, and the boride and the phosphide have a synergistic flame-retardant effect, so that the flame-retardant effect is enhanced, the combustion rate of the material is effectively reduced, and the micron-sized organic silicon light diffusant has the beneficial effect of flame-retardant property.
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Description

Technical Field

[0001] The invention relates to the technical field of organic silicon, in particular to a flame-retardant micron-sized organic silicon light diffuser and a preparation process thereof. Background Art

[0002] The most widely used lens materials for LED lamps include polycarbonate, polymethyl methacrylate and glass. These materials mixed with some light diffusers can obtain advantages such as higher transparency and light intensity suitable for human eyes. However, with the advancement of science and technology, the strength and linear expansion coefficient of these materials themselves are increasingly unable to meet the requirements, especially for long, thin, soft and wide LED lamps. The bending performance, contraction or expansion performance of these materials are far from meeting the standards. Therefore, for long, thin, soft and wide LED lamps, another soft elastic packaging material - potting material is favored by the market. Potting materials mainly include epoxy resin and silicone material. Because epoxy resin will change color and cannot withstand high-temperature welding process, its application also has certain limitations. Therefore, the most promising material at present is silicone material. Silicone material can absorb heat and prevent discoloration, especially it has a higher refractive index. The only drawback is that the haze of silicone material is generally low.

[0003] In order to solve the defects of the prior art, a light-diffusing organic silicon composite material and a preparation method thereof are disclosed with publication number CN 113667306 B. The technical scheme enables the organic silicon material to maintain a high light transmittance; at the same time, because the refractive index of these light diffusers is greater than 1.45, and the refractive index of the base glue used is generally 1.39-1.40, after the potting glue is cured, the light diffuser and the polydimethylsiloxane are phase-separated at the microscopic level, giving the potting glue a higher haze.

[0004] The light diffuser in the material is liquid and contains groups with high molar refractive index, which can reduce the loss of transmitted light and maintain high transmittance. However, the light diffuser is liquid and contains groups with high molar refractive index: ether bonds, aromatic rings, and alkoxy groups that hydrolyze to produce ester bonds with high molar refractive index. The high molar refractive index groups in the light diffuser, such as aromatic rings and ether bonds, will affect the combustion characteristics of the material. Summary of the invention

[0005] Technical issues solved:

[0006] In view of the deficiencies in the prior art, the present invention provides a flame-retardant micron-sized organosilicon light diffuser and a preparation process thereof. The prepared organosilicon light diffuser has the advantages of flame retardancy and stable performance, which makes up for the problem of insufficient flame retardancy of the existing light diffusers and solves the above-mentioned technical problems.

[0007] Technical solution:

[0008] To achieve the above-mentioned purpose, the present invention provides the following technical scheme: the first step is to synthesize an organosilicon core by hydrolyzing siloxane and then polycondensing it, emulsifying the synthesized organosilicon light diffuser core into a uniform system, adding boric acid and ammonium tripolyphosphate to modify the surface of the organosilicon core, and finally obtaining an organosilicon light diffuser with flame retardant function by post-treatment.

[0009] Preferably, the organosilane is methyltrimethoxysilane or phenyltrimethoxysilane, and the mass ratio of pure water to the organosilane during hydrolysis is 3:1-10:1.

[0010] Preferably, the pH regulator is one of dilute hydrochloric acid or tetramethylammonium hydroxide solution.

[0011] Preferably, the nonionic emulsifier is one of AEO3 and OP-10 or a mixture thereof, and the added amount is 10%-25% of the mass of the pH regulator.

[0012] A flame retardant silicone light diffuser preparation process, synthesis of silicone core:

[0013] S1.1. Add deionized water into a three-necked glass flask with heating and stirring;

[0014] S1.2, add the measured organosilane into a three-necked flask;

[0015] S1.3, adjust the pH of the system in the three-necked flask with dilute hydrochloric acid to between 3-4;

[0016] S1.4, slowly raise the temperature to 40-60°C, and stir at constant temperature for 0.5-3 hours;

[0017] S1.5, then add tetramethylammonium hydroxide as a polycondensation catalyst to carry out a polycondensation reaction, and the pH of the polycondensation system is between 8-10;

[0018] S1.6, after adding the polycondensation catalyst, stop stirring and keep the polymerization statically for 2-4 hours;

[0019] S1.7, after the polycondensation is completed, non-ionic emulsifiers AEO3 and OP-10 are added to increase the viscosity of the system through emulsification, so that the system becomes a uniform dispersion system;

[0020] Step 2: Modification:

[0021] S2.1, mixing the boride and the phosphide in proportion, adding them to the uniform system in S1.7 in proportion, stirring evenly, and performing surface modification on the organosilicon microspheres;

[0022] S2.2, the reaction temperature is 30-50°C, and the reaction time is 1-3 hours;

[0023] Step 3: Purification:

[0024] S3.1, cooling the mixture to room temperature, and performing physical separation by centrifugation at a speed of 2500-4500 rpm;

[0025] S3.2. Wash the centrifuged reactants with pure water 1-2 times to clean the products;

[0026] S3.3, drying the cleaned product in an oven;

[0027] S3.4, grinding and sieving the dried material to obtain a flame retardant micron-sized organic silicon light diffuser;

[0028] S3.5. The particle size of the product was analyzed by laser particle size analyzer, and the appearance and sphericity of the product were analyzed by scanning electron microscope.

[0029] Deionized water is used as a solvent to avoid the use of organic solvents and reduce environmental pollution. By adjusting parameters such as pH value, temperature and reaction time, the synthesis and modification process of the silicone core can be precisely controlled to obtain a flame-retardant micron-sized silicone light diffuser with specific properties. Emulsification technology is used to increase the viscosity of the system so that the silicone microspheres are evenly dispersed in the system, thereby improving the reaction efficiency. Borides and phosphides are introduced into the surface of the silicone microspheres through surface modification, thereby improving the stability and flame retardancy of the product. The particle size can be precisely controlled by analyzing the particle size with a laser particle size analyzer to meet the needs of different application scenarios. The appearance and sphericity of the product are analyzed with a scanning electron microscope to ensure that the product has a good appearance and sphericity, which is beneficial to its application in the optical field.

[0030] Preferably, the temperature of the three-necked flask in step 1 is raised to 45-60°C, the polycondensation catalyst is added dropwise at a rate of 3-5 drops per minute, and the pH range of the system set in step 1 is expressed as: pH 初 (Initial): 3≤pH 初 ≤4.

[0031] Preferably, the temperature increase process in step 1 is expressed as: T 升温 (Temperature): 45℃≤T 升温 ≤60℃,t 搅拌 (Stirring time): 0.5 hours ≤ t 搅拌 ≤3 hours.

[0032] Preferably, the reaction temperature in step 2 is expressed as: 30°C ≤ T 反应 ≤50℃;

[0033] The reaction time expression is: 1 hour ≤ t 反应 ≤3 hours.

[0034] Preferably, the physical separation expression in step three is: centrifugal speed: 2500 rpm ≤ speed ≤ 4500 rpm.

[0035] Preferably, the cleaning expression in step three is: number of cleaning times: 1 time ≤ number of cleaning times ≤ 2 times.

[0036] Compared with the prior art, the present invention provides a flame-retardant micron-sized organic silicon light diffuser and a preparation process thereof, which has the following beneficial effects:

[0037] 1. The present invention improves the flame retardancy of the material by introducing special flame retardant components: boric acid and ammonium tripolyphosphate on the surface of the organosilicon light diffuser. The organosilicon light diffuser is selected to have good chemical stability and good synergy with other components. The pH value of the system is adjusted between 3-4 to ensure the smooth progress of the hydrolysis reaction of the organosiloxane. The pH value of the polycondensation reaction is between 8-10, which optimizes the reaction conditions and improves the uniformity and quality of the product. Boride and phosphide are added in the modification step: the mixture of boride and phosphide further enhances the flame retardant effect. Boride and phosphide have a synergistic effect and can effectively reduce the combustion rate of the material, achieving the beneficial effect of the organosilicon light diffuser having excellent flame retardancy.

[0038] 2. The present invention uses polycondensation siloxane. This organic silicon core has excellent stability and reactivity and can provide a stable basic structure. AEO3 and OP-10 help to form a uniform dispersion system, improve the stability of the mixture, prevent the stratification or precipitation of the components, and accurately control the pH value of the system at different stages. The initial pH value is controlled between 3-4, and the condensation reaction stage is maintained between 8-10, which ensures the smooth progress of the chemical reaction and optimizes the structure and performance of the final product. The reaction temperature is within the range of 40-60°C, and the reaction time is controlled within the range of 0.5 to 3 hours, ensuring the uniformity of the reaction and the consistency of the reaction products. In step 2, the boride and the phosphide are mixed in proportion and added to the system for modification. This step ensures the effectiveness of the modification process by adjusting the temperature to 30-50°C and the time to 1-3 hours, so that the surface modification of the organic silicon microspheres is uniform, and the stability and performance of the product are enhanced. The reactants are separated by centrifugation at 2500-4500 rpm and washed with pure water 1-2 times to remove impurities and unreacted substances, improve the purity and stability of the product, and achieve the beneficial effect of stable performance of the prepared organic silicon light diffuser. BRIEF DESCRIPTION OF THE DRAWINGS

[0039] Figure 1 It is a schematic diagram of the process steps of the present invention;

[0040] Figure 2 Product SEM analysis diagram;

[0041] Figure 3 Product laser particle size analyzer particle size analysis spectrum. DETAILED DESCRIPTION

[0042] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. 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.

[0043] See also Figure 1 , a flame-retardant silicone light diffuser. The first step is to synthesize a silicone core by hydrolyzing siloxane and then polycondensing it. After the synthesized silicone light diffuser core is emulsified into a uniform system, boric acid and ammonium tripolyphosphate are added to modify the surface of the silicone core. Finally, a silicone light diffuser with flame-retardant function is obtained by post-treatment.

[0044] The invention introduces special flame retardant components: boric acid and ammonium tripolyphosphate on the surface of the organosilicon light diffuser, thereby improving the flame retardancy of the material. The organosilicon light diffuser is selected to have good chemical stability and good synergy with other components.

[0045] The pH value of the system is adjusted between 3-4 to ensure the stability of the silicone and the smooth progress of the reaction. The pH value of the polycondensation reaction is between 8-10, which optimizes the reaction conditions and improves the uniformity and quality of the product. Borides and phosphides are added in the modification step: the mixture of borides and phosphides further enhances the flame retardant effect. Borides and phosphides have a synergistic effect and can effectively reduce the burning rate of the material.

[0046] Specifically, the organosilane is methyltrimethoxysilane or phenyltrimethoxysilane, and the mass ratio of pure water to the organosilane during hydrolysis is 3:1-10:1.

[0047] Specifically, the pH regulator is one of dilute hydrochloric acid or tetramethylammonium hydroxide solution.

[0048] Specifically, the nonionic emulsifier is one of AEO3 and OP-10 or a mixture thereof, and the added amount is 10%-25% of the mass of the pH regulator.

[0049] A flame retardant organic silicon light diffuser preparation process, the preparation process consists of the following steps:

[0050] S1.1. Add deionized water into a three-necked glass flask with heating and stirring;

[0051] S1.2, add the measured organosilane into a three-necked flask;

[0052] S1.3, adjust the pH of the system in the three-necked flask with dilute hydrochloric acid to between 3-4;

[0053] S1.4, slowly raise the temperature to 40-60°C, and stir at constant temperature for 0.5-3 hours;

[0054] S1.5, then add tetramethylammonium hydroxide as a polycondensation catalyst to carry out a polycondensation reaction, and the pH of the polycondensation system is between 8-10;

[0055] S1.6, after adding the polycondensation catalyst, stop stirring and keep the polymerization statically for 2-4 hours;

[0056] S1.7, after the polycondensation is completed, non-ionic emulsifiers AEO3 and OP-10 are added to increase the viscosity of the system through emulsification, so that the system becomes a uniform dispersion system;

[0057] Step 2: Modification:

[0058] S2.1, mixing the boride and the phosphide in proportion, adding them to the uniform system in S1.7 in proportion, stirring evenly, and performing surface modification on the organosilicon microspheres;

[0059] S2.2, the reaction temperature is 30-50°C, and the reaction time is 1-3 hours;

[0060] Step 3: Purification:

[0061] S3.1, cooling the mixture to room temperature, and performing physical separation by centrifugation at a speed of 2500-4500 rpm;

[0062] S3.2. Wash the centrifuged reactants with pure water 1-2 times to clean the products;

[0063] S3.3, drying the cleaned product in an oven;

[0064] S3.4, grinding and sieving the dried material to obtain a flame retardant micron-sized organic silicon light diffuser;

[0065] S3.5. The particle size of the product was analyzed by laser particle size analyzer, and the appearance and sphericity of the product were analyzed by scanning electron microscope.

[0066] Methylsilane is used. This organosilane has excellent performance in stability and reactivity and can provide a stable basic structure. AEO3 and OP-10 help to form a uniform dispersion system, improve the stability of the mixture, prevent stratification or precipitation of components, and accurately control the pH value of the system at different stages. The initial pH value is controlled between 3-4, and the condensation reaction stage is maintained between 8-10, ensuring the smooth progress of the chemical reaction and optimizing the structure and performance of the final product. The reaction temperature is in the range of 40-60°C, and the reaction time is controlled between 0.5 and 3 hours, ensuring the uniformity of the reaction and the consistency of the reaction product. In step 2, the boride and the phosphide are mixed in proportion and added to the system for modification. This step ensures the effectiveness of the modification process by adjusting the temperature to 30-50°C and the time to 1-3 hours, so that the surface modification of the organosilicon microspheres is uniform, and the stability and performance of the product are enhanced. The reactants are separated by centrifugation at 2500-4500 rpm and washed with pure water 1-2 times to remove impurities and unreacted substances, thereby improving the purity and stability of the product.

[0067] Specifically, in step 1, the temperature of the three-necked flask is raised to 45-60°C, and the polycondensation catalyst is added dropwise at a rate of 3-5 drops per minute. The pH range of the system set in step 1 is expressed as: pH 初 (Initial): 3≤pH 初 ≤4.

[0068] Specifically, the temperature rise process in step 1 is expressed as: T 升温 (Temperature): 45℃≤T 升温 ≤60℃,t 搅拌 (Stirring time): 0.5 hours ≤ t 搅拌 ≤3 hours.

[0069] Specifically, the reaction temperature in step 2 is expressed as: 30°C ≤ T 反应 ≤50℃;

[0070] The reaction time expression is: 1 hour ≤ t 反应 ≤3 hours.

[0071] Specifically, the physical separation expression in step three is: centrifugal speed: 2500 rpm ≤ speed ≤ 4500 rpm.

[0072] Specifically, the cleaning expression in step three is: number of cleaning times: 1 time ≤ number of cleaning times ≤ 2 times.

[0073] Embodiment 1

[0074] Raw material ratio:

[0075] Organosilane: methyltrimethoxysilane 30 g;

[0076] Deionized water: 300 ml;

[0077] Dilute hydrochloric acid: appropriate amount (adjust pH to 3.5);

[0078] Tetramethylammonium hydroxide: 0.5 g;

[0079] Non-ionic emulsifier: AEO3 1g + OP-10 2g;

[0080] Boride: 0.6 g;

[0081] Phosphide: 0.4 g;

[0082] Preparation steps:

[0083] Hydrolysis reaction: Add 30 g of methyltrimethoxysilane and 300 ml of deionized water to the reaction vessel and start stirring. Slowly add dilute hydrochloric acid, keep stirring, and adjust the pH to 3.5;

[0084] Reaction conditions: Stir continuously for 2 hours at 50°C to fully hydrolyze the organosilane;

[0085] Emulsification: Add 1g AEO3 and 2g OP-10, continue stirring, maintain the temperature and stirring speed, until a uniform emulsion is formed;

[0086] Modification: Add 0.6 g of boride and 0.4 g of phosphide and react for 2 hours to modify the product;

[0087] Centrifugation: After completion, transfer the reaction mixture to a centrifuge, set at 3000 rpm, and centrifuge for 15 minutes to separate the solid and liquid;

[0088] Washing: Wash the precipitate twice with deionized water to remove excess emulsifier;

[0089] Drying: Place the washed precipitate in a 50°C oven and dry to constant weight to obtain the final product.

[0090] Embodiment 2

[0091] Raw material ratio:

[0092] Organosilane: phenyltrimethoxysilane 40 g;

[0093] Deionized water: 400 ml;

[0094] Dilute hydrochloric acid: appropriate amount (adjust pH to 3.2);

[0095] Tetramethylammonium hydroxide: 0.6 g;

[0096] Non-ionic emulsifier: AEO3 2g + OP-10 1g;

[0097] Boride: 0.8 g;

[0098] Phosphide: 0.2 g;

[0099] Preparation steps:

[0100] Hydrolysis reaction: In a reaction vessel, add 40 g of phenyltrimethoxysilane and 400 ml of deionized water and adjust the pH to 3.2;

[0101] Temperature control: The reaction temperature was controlled at 45°C and stirred for 1 hour to ensure the hydrolysis reaction;

[0102] Emulsification and modification reaction: Add AEO3 and OP-10, maintain stirring, add 0.8g of boride and 0.2g of phosphide at the same time, and react for 3 hours;

[0103] Separation: centrifugation and washing are performed as in Example 1;

[0104] Drying: Dry in an oven at 50°C to constant weight to obtain the product;

[0105] Embodiment 3

[0106] Raw material ratio:

[0107] Organosilane: 50 g methyltriethoxysilane;

[0108] Deionized water: 250 ml;

[0109] Dilute hydrochloric acid: appropriate amount (adjust pH to 3.7);

[0110] Tetramethylammonium hydroxide: 0.7 g;

[0111] Nonionic emulsifier: AEO3 1.5g + OP-10 1.5g;

[0112] Boride: 0.5 g;

[0113] Phosphide: 0.5 g;

[0114] Preparation steps:

[0115] Mixing and hydrolysis: Mix 50 g of methyltriethoxysilane with 250 ml of deionized water, adjust the pH to 3.7, and stir well;

[0116] Reaction heating: Heat to 55°C and stir the reaction for 1.5 hours to ensure hydrolysis;

[0117] Emulsification: Add 1.5 g AEO3 and 1.5 g OP-10, add 0.5 g boride and 0.5 g phosphide at the same time, and set the reaction time to 1 hour;

[0118] Separation: Centrifuge at 4000 rpm for 15 minutes;

[0119] Cleaning: Wash the precipitate once with deionized water to remove impurities, and then put the product into an oven to dry.

[0120] Embodiment 4

[0121] Raw material ratio:

[0122] Organosilane: phenyltriethoxysilane 35 g;

[0123] Deionized water: 350 ml;

[0124] Dilute hydrochloric acid: appropriate amount (adjust pH to 4.0);

[0125] Tetramethylammonium hydroxide: 0.4 g;

[0126] Nonionic emulsifier: AEO3 1g + OP-10 3g;

[0127] Boride: 0.7 g;

[0128] Phosphide: 0.3 g;

[0129] Preparation steps:

[0130] Hydrolysis reaction: Mix 35 g of phenyltriethoxysilane with 350 ml of deionized water in a reaction vessel and adjust the pH to 4.0;

[0131] Reaction control: Stir at 50°C for about 2.5 hours to ensure the reaction is complete;

[0132] Emulsification reaction: add AEO3 and OP-10, continue stirring, add 0.7 g of boride and 0.3 g of phosphide for modification reaction for 2 hours;

[0133] Centrifugation and washing: Separate the solids from the liquid by centrifuge and wash twice;

[0134] Drying: Dry in an oven at 50°C to constant weight.

[0135] Embodiment 5

[0136] Raw material ratio:

[0137] Organosilane: methyltrimethoxysilane 60 g;

[0138] Deionized water: 300 ml;

[0139] Dilute hydrochloric acid: appropriate amount (adjust pH to 3.3);

[0140] Tetramethylammonium hydroxide: 0.5 g;

[0141] Nonionic emulsifier: AEO3 2g + OP-10 2g;

[0142] Boride: 0.6 g;

[0143] Phosphide: 0.4 g;

[0144] Preparation steps:

[0145] Hydrolysis reaction: 60 g of methyltrimethoxysilane and 300 ml of deionized water were added to the reactor and the pH was adjusted to 3.3;

[0146] Reaction conditions: Stir at 45°C for 3 hours to promote the hydrolysis reaction;

[0147] Modified emulsification: Add AEO3 and OP-10, keep stirring and add boride and phosphide, the reaction time is established as 3 hours;

[0148] Centrifugation: Set to 4500 rpm for 15 minutes to separate solids;

[0149] Cleaning and drying: Clean twice with deionized water and finally dry in an oven to constant weight.

[0150] project index Example 1 Example 2 Example 3 <![CDATA[Particle size a (Dv 50 ), μm]]> 5~8 5.6 6.8 6.2 span ≤1.4 0.94 1.02 0.98 Moisture,% ≤1.0 0.5 0.6 0.5 Thermal weight loss, % ≤2.0 1.0 0.9 1.1 pH 5~8 6 7 6

[0151] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A flame retardant silicone light diffuser, characterized in that: The micron-sized organosilicon core is prepared by hydrolyzing siloxane and then polycondensing it. After the synthesized organosilicon light diffuser core is emulsified into a uniform system, boric acid and ammonium tripolyphosphate are added to modify the surface of the organosilicon core. Finally, the organosilicon light diffuser with flame retardant function is obtained by post-treatment.

2. The flame retardant organic silicon light diffuser according to claim 1, characterized in that: The organosilane is methyltrimethoxysilane or phenyltrimethoxysilane, and the mass ratio of pure water to the organosilane during hydrolysis is 3:1-10:

1.

3. The flame retardant organosilicon light diffuser according to claim 1, characterized in that: The pH regulator is one of dilute hydrochloric acid or tetramethylammonium hydroxide solution.

4. The flame retardant organic silicon light diffuser according to claim 2, characterized in that: The nonionic emulsifier is one of AEO3 and OP-10 or a mixture thereof, and the added amount is 10%-25% of the mass of the pH regulator according to claim 2.

5. A process for preparing a flame retardant organic silicon light diffusing agent, characterized in that: The preparation process is used for the diffusing agent according to claim 1, and the preparation process consists of the following steps: Step 1: Synthesis of silicone core: S1.

1. Add deionized water into a three-necked glass flask with heating and stirring; S1.2, add the measured organosilane into a three-necked flask; S1.3, adjust the pH of the system in the three-necked flask with dilute hydrochloric acid to between 3-4; S1.4, slowly raise the temperature to 40-60°C, and stir at constant temperature for 0.5-3 hours; S1.5, then add tetramethylammonium hydroxide as a polycondensation catalyst to carry out a polycondensation reaction, and the pH of the polycondensation system is between 8-10; S1.6, after adding the polycondensation catalyst, stop stirring and keep the polymerization statically for 2-4 hours; S1.7, after the polycondensation is completed, non-ionic emulsifiers AEO3 and OP-10 are added to increase the viscosity of the system through emulsification, so that the system becomes a uniform dispersion system; Step 2: Modification: S2.1, mixing the boride and the phosphide in proportion, adding them to the uniform system in S1.7 in proportion, stirring evenly, and performing surface modification on the organosilicon microspheres; S2.2, the reaction temperature is 30-50°C, and the reaction time is 1-3 hours; Step 3: Purification: S3.1, cooling the mixture to room temperature, and performing physical separation by centrifugation at a speed of 2500-4500 rpm; S3.

2. Wash the centrifuged reactants with pure water 1-2 times to clean the products; S3.3, drying the cleaned product in an oven; S3.4, grinding and sieving the dried material to obtain a flame retardant micron-sized organic silicon light diffuser; S3.

5. The particle size of the product was analyzed by laser particle size analyzer, and the appearance and sphericity of the product were analyzed by scanning electron microscope.

6. The process for preparing a flame retardant organic silicon light diffusing agent according to claim 5, characterized in that: In the step 1, the temperature of the three-necked flask is raised to 45-60°C, and the polycondensation catalyst is added dropwise at a rate of 3-5 drops per minute. The pH range of the system in the step 1 is set as follows: pH 初 (Initial): 3≤pH 初 ≤4.

7. The process for preparing a flame retardant organic silicon light diffusing agent according to claim 5, characterized in that: The temperature rise process in step 1 is expressed as: T 升温 (Temperature): 45℃≤T 升温 ≤60℃,t 搅拌 (Stirring time): 0.5 hours ≤ t 搅拌 ≤3 hours.

8. The process for preparing a flame retardant organic silicon light diffusing agent according to claim 5, characterized in that: The reaction temperature in step 2 is expressed as: 30°C≤T 反应 ≤50℃; The reaction time expression is: 1 hour ≤ t 反应 ≤3 hours.

9. The process for preparing a flame retardant organic silicon light diffusing agent according to claim 5, characterized in that: The physical separation expression in step three is: centrifugal speed: 2500 rpm≤speed≤4500 rpm.

10. The process for preparing a flame retardant organic silicon light diffusing agent according to claim 5, characterized in that: The cleaning expression in step 3 is: number of cleaning times: 1 time ≤ number of cleaning times ≤ 2 times.

Citation Information

Patent Citations

  • A light-diffusing organosilicon composite material and its preparation method

    CN113667306B