Perlite particles and preparation method thereof
By combining perlite with modified silica aerogel, coconut oil, palmitic acid and modified microcrystalline wax, perlite particles with excellent insulation, waterproof, flame retardant and mechanical properties were prepared, solving the problem of insufficient performance of expanded perlite in the field of insulation and heat insulation.
Patent Information
- Application Number
- CN202411925255.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-25
- Publication Date
- 2025-05-13
AI Technical Summary
Expanded perlite is widely used in the field of thermal insulation, but it is easy to absorb moisture, has a large thermal conductivity, and has a small compressive strength, making it difficult to meet the needs of high-performance thermal insulation materials.
Perlite particles with excellent thermal insulation, waterproofing, flame retardant and mechanical properties were prepared by combining perlite with modified silica aerogel, coconut oil, palmitic acid and modified microcrystalline wax.
It has achieved the improvement of the insulation performance of perlite particles, enhanced waterproof performance, improved flame retardant performance and improved mechanical performance, meeting the needs of high-performance insulation materials.
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of perlite materials, and in particular to perlite particles and a preparation method thereof. Background Art
[0002] Perlite is a glassy rock formed by the rapid cooling of acidic lava from volcanic eruptions. It is named for its pearly fissure structure. Expanded perlite is a commonly used inorganic lightweight aggregate for thermal insulation. It has many advantages such as light weight, high porosity, non-combustibility, and the same life cycle as the building. It is widely used in the field of thermal insulation. However, compared with organic thermal insulation materials, expanded perlite is easy to absorb moisture, has a relatively large thermal conductivity, and has low compressive strength. Summary of the invention
[0003] Based on the technical problems existing in the background technology, the present invention proposes a perlite particle and a preparation method thereof.
[0004] The invention provides perlite particles, which include perlite, modified silica aerogel, coconut oil, palmitic acid and modified microcrystalline wax.
[0005] Preferably, the perlite is expanded perlite, and the particle size of the perlite is 0.5-5 mm.
[0006] Preferably, the method for preparing the modified silica aerogel comprises the following steps:
[0007] S1, water glass and water are mixed evenly, and then subjected to resin exchange, hydrolysis and alkali catalysis to obtain wet gel;
[0008] S2, aging, replacement modification and drying the wet gel to obtain the product.
[0009] More preferably, in said S1, the volume ratio of water glass to water is 1:(3-6).
[0010] More preferably, in said S1, the resin is a cation exchange resin.
[0011] More preferably, in S1, the substance added in the hydrolysis process is selected from one or more of formamide, N,N-dimethylformamide, hydrochloric acid and nitric acid.
[0012] More preferably, in the S1, an alkali catalyst is added to adjust the pH to 5-7.
[0013] More preferably, in said S1, the base catalyst is aqueous ammonia.
[0014] More preferably, in said S2, aging comprises soaking the wet gel in an aging solution for 10-30 hours.
[0015] More preferably, the aging liquid is selected from an ethanol aqueous solution and an ethanol-ethyl orthosilicate mixed solution.
[0016] More preferably, the volume fraction of the ethanol aqueous solution is 10-25%.
[0017] More preferably, the molar ratio of ethanol to tetraethyl orthosilicate in the ethanol-tetraethyl orthosilicate mixed solution is (3-4):1.
[0018] More preferably, in said S2, the replacement modification comprises soaking the aged wet gel in a modifier for 10-30 hours.
[0019] More preferably, the modifier includes trimethylchlorosilane, n-heptane, and ethanol.
[0020] More preferably, the volume ratio of trimethylsilyl chloride, n-heptane and ethanol is 1:(1.2-1.5):(0.1-0.5).
[0021] More preferably, in said S2, the drying is drying at normal pressure.
[0022] More preferably, in said S2, drying comprises drying at 40-60° C. for 6-10 h.
[0023] Preferably, the preparation method of the modified microcrystalline wax comprises the following steps: adding carbon nanotubes to the microcrystalline wax under temperature conditions T1, ultrasonic treatment, and heating and stirring uniformly under temperature conditions T2 to obtain the modified microcrystalline wax.
[0024] More preferably, the T1 temperature is 85-95°C.
[0025] More preferably, the molecular weight of the microcrystalline wax is 500-700.
[0026] More preferably, the mass ratio of the microcrystalline wax to the carbon nanotubes is 100:(0.1-0.5).
[0027] More preferably, the frequency of the ultrasonic treatment is 20-40 kHz, and the time of the ultrasonic treatment is 1-2 h.
[0028] More preferably, the T2 temperature is 60-70°C.
[0029] More preferably, the rotation speed is 50-200 r / min.
[0030] The present invention also provides a method for preparing pearlite particles, comprising the following steps:
[0031] S1, pretreating the perlite to obtain pretreated perlite;
[0032] S2, heating and mixing the coconut oil, palmitic acid and modified microcrystalline wax to obtain a mixture;
[0033] S3, mixing the pretreated perlite, the mixture and the modified silica aerogel, and performing vacuum heating treatment to obtain.
[0034] Preferably, in S1, the pretreatment comprises adding water to the perlite, stirring, standing, and heating to obtain the perlite.
[0035] More preferably, the volume ratio of perlite to water is 1:(5-10).
[0036] More preferably, the heating treatment comprises first keeping the temperature at 100-110° C. for 1-2 hours, and then keeping the temperature at 200-300° C. for 5-20 minutes.
[0037] Pre-treating the perlite is helpful for combining the perlite with the mixture and modified silica aerogel in the subsequent process.
[0038] Preferably, in S2, the mass ratio of coconut oil, palmitic acid and modified microcrystalline wax is 14:(0.4-0.5):(0.8-1).
[0039] Preferably, in said S2, the heating temperature is 70-95°C.
[0040] Preferably, in S3, the mass ratio of the mixture, the pretreated perlite and the modified silica aerogel is (0.1-2):1:(1-10).
[0041] Preferably, in said S3, the vacuum heating treatment comprises heating at 0.02-1 MPa and 60-80° C. for 0.5-3 h.
[0042] Preferably, in the above S3, the step of introducing a protective gas is further included before the vacuum heating treatment.
[0043] More preferably, the protective gas is selected from one or more of nitrogen and argon.
[0044] The beneficial effects of the present invention are:
[0045] The perlite particles provided by the present invention include perlite, modified silica aerogel, coconut oil, palmitic acid, and modified microcrystalline wax. The raw materials act synergistically, and the obtained perlite particles have excellent thermal insulation, waterproof, flame retardant and mechanical properties. DETAILED DESCRIPTION
[0046] The technical solution of the present invention is described in detail through specific embodiments.
[0047] Unless otherwise specified, the materials and reagents used in the following examples can be obtained from commercial sources.
[0048] Example 1
[0049] A method for preparing perlite particles comprises the following steps:
[0050] S1. Add water to the expanded perlite and stir for 5 minutes, let it stand for 30 minutes, take the expanded perlite on the water surface and dry it at 105°C for 2 hours, and then keep it at 300°C for 10 minutes to obtain pretreated perlite;
[0051] S2, heating and mixing coconut oil, palmitic acid and modified microcrystalline wax at a mass ratio of 14:0.5:0.9 at 90°C to obtain a mixture; the preparation method of modified microcrystalline wax comprises the following steps: adding 0.2% carbon nanotubes to molten microcrystalline wax at 90°C, ultrasonically treating at 25kHz for 1h, heating and stirring at 65°C and 80r / min to obtain a mixture;
[0052] S3. The mixture, pretreated perlite and modified silica aerogel are mixed in a mass ratio of 0.5:1:2, and vacuum heated at 0.5 MPa and 75° C. for 1 h to obtain the obtained product.
[0053] The preparation method of modified silica aerogel comprises the following steps:
[0054] S1, water glass and water were mixed evenly in a volume ratio of 1:4, exchanged with styrene cation exchange resin, added with formamide and hydrochloric acid to adjust the pH to 2, hydrolyzed for 12 hours, added with 1 mol / L ammonia alkali catalysis, adjusted the pH to 6, and obtained a wet gel;
[0055] S2. The wet gel is added to an ethanol-ethyl orthosilicate mixed solution (the molar ratio of ethanol to ethyl orthosilicate is 3:1) and aged for 24 hours. The aged wet gel is immersed in a mixed solution of trimethylchlorosilane, n-heptane and ethanol in a volume ratio of 1:1.5:0.25 for replacement modification for 24 hours. The gel is dried at 60°C under normal pressure for 8 hours.
[0056] Example 2
[0057] A method for preparing perlite particles comprises the following steps:
[0058] S1. Add water to the expanded perlite and stir for 5 minutes, let it stand for 25 minutes, take the expanded perlite on the water surface and dry it at 110°C for 1.5 hours, and then keep it at 300°C for 10 minutes to obtain pretreated perlite;
[0059] S2, heating and mixing coconut oil, palmitic acid and modified microcrystalline wax at a mass ratio of 15:0.5:1 at 90°C to obtain a mixture; the preparation method of modified microcrystalline wax comprises the following steps: adding 0.15% carbon nanotubes to molten microcrystalline wax at 90°C, ultrasonically treating at 30kHz for 1h, and heating and stirring at 65°C and 100r / min to obtain a mixture;
[0060] S3. The mixture, pretreated perlite and modified silica aerogel are mixed in a mass ratio of 0.6:1:2, and subjected to vacuum heating treatment at 0.5 MPa and 65° C. for 0.5 h to obtain the product.
[0061] The preparation method of modified silica aerogel comprises the following steps:
[0062] S1, water glass and water were mixed evenly in a volume ratio of 1:3, exchanged with styrene cation exchange resin, added with formamide and hydrochloric acid to adjust the pH to 2, hydrolyzed for 12 hours, added with 1 mol / L ammonia alkali catalysis, adjusted the pH to 6, and obtained a wet gel;
[0063] S2. The wet gel is added to an ethanol-ethyl orthosilicate mixed solution (the molar ratio of ethanol to ethyl orthosilicate is 4:1) and aged for 24 hours. The aged wet gel is immersed in a mixed solution of trimethylchlorosilane, n-heptane and ethanol in a volume ratio of 1:1.3:0.2 for replacement modification for 24 hours. The gel is dried at normal pressure at 60°C for 8 hours.
[0064] Example 3
[0065] A method for preparing perlite particles comprises the following steps:
[0066] S1. Add water to the expanded perlite and stir for 5 minutes, let it stand for 30 minutes, take the expanded perlite on the water surface and dry it at 105°C for 2 hours, and then keep it at 300°C for 10 minutes to obtain pretreated perlite;
[0067] S2, heating and mixing coconut oil, palmitic acid and modified microcrystalline wax at a mass ratio of 14:0.4:0.9 at 90°C to obtain a mixture; the preparation method of modified microcrystalline wax comprises the following steps: adding 0.25% carbon nanotubes to molten microcrystalline wax at 90°C, ultrasonically treating at 35kHz for 1h, heating and stirring at 65°C and 150r / min to obtain a mixture;
[0068] S3. The mixture, pretreated perlite and modified silica aerogel are mixed in a mass ratio of 0.4:1:2, and subjected to vacuum heating treatment at 0.5 MPa and 75° C. for 1 h to obtain the product.
[0069] The preparation method of modified silica aerogel comprises the following steps:
[0070] S1, water glass and water were mixed evenly in a volume ratio of 1:3, exchanged with styrene cation exchange resin, added with formamide and hydrochloric acid to adjust the pH to 2, hydrolyzed for 12 hours, added with 1 mol / L ammonia alkali catalysis, adjusted the pH to 7, and obtained a wet gel;
[0071] S2. The wet gel is added to an ethanol-ethyl orthosilicate mixed solution (the molar ratio of ethanol to ethyl orthosilicate is 3:1) and aged for 24 hours. The aged wet gel is immersed in a mixed solution of trimethylchlorosilane, n-heptane and ethanol in a volume ratio of 1:1.2:0.2 for replacement modification for 24 hours. The gel is dried at normal pressure at 60°C for 8 hours.
[0072] Example 4
[0073] A method for preparing perlite particles comprises the following steps:
[0074] S1. Add water to the expanded perlite and stir for 5 minutes, let it stand for 30 minutes, take the expanded perlite on the water surface and dry it at 105°C for 2 hours, and then keep it at 300°C for 10 minutes to obtain pretreated perlite;
[0075] S2, heating and mixing coconut oil, palmitic acid and modified microcrystalline wax at a mass ratio of 14:0.5:0.9 at 90°C to obtain a mixture; the preparation method of modified microcrystalline wax comprises the following steps: adding 0.15% carbon nanotubes to molten microcrystalline wax at 95°C, ultrasonically treating at 30kHz for 1h, heating and stirring at 60°C and 200r / min to obtain a mixture;
[0076] S3. The mixture, pretreated perlite and modified silica aerogel are mixed in a mass ratio of 0.6:1:2, and vacuum heated at 0.5 MPa and 75° C. for 1 h to obtain the product.
[0077] The preparation method of modified silica aerogel comprises the following steps:
[0078] S1, water glass and water were mixed evenly in a volume ratio of 1:4, exchanged with styrene cation exchange resin, added with formamide and hydrochloric acid to adjust the pH to 2, hydrolyzed for 12 hours, added with 1 mol / L ammonia alkali catalysis, adjusted the pH to 6, and obtained a wet gel;
[0079] S2. The wet gel is added to an ethanol-ethyl orthosilicate mixed solution (the molar ratio of ethanol to ethyl orthosilicate is 3:1) and aged for 24 hours. The aged wet gel is immersed in a mixed solution of trimethylchlorosilane, n-heptane and ethanol in a volume ratio of 1:1.2:0.3 for replacement modification for 24 hours, and dried at 60°C under normal pressure for 8 hours.
[0080] The above perlite particles were tested for water absorption, thermal conductivity, compressive strength, and combustion performance. The test results are shown in Table 1.
[0081] Table 1
[0082] project Water absorption (%) Thermal conductivity (W / m·K) Compressive strength(MPa) Combustion performance Example 1 3.8 0.020 0.46 A1 Example 2 3.5 0.018 0.47 A1 Example 3 3.9 0.020 0.46 A1 Example 4 3.6 0.019 0.46 A1
[0083] In summary, the perlite particles provided by the present invention have excellent thermal insulation, waterproof, flame retardant and mechanical properties.
[0084] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.
Claims
1. A perlite particle comprising perlite, modified silica aerogel, coconut oil, palmitic acid, and modified microcrystalline wax.
2. The pearlite particles according to claim 1, characterized in that The preparation method of the modified silica aerogel comprises the following steps: S1, mixing water glass and water evenly, and then performing resin exchange, hydrolysis and alkali catalysis to obtain a wet gel; S2, aging, replacement modification and drying the wet gel to obtain the modified silica aerogel.
3. The pearlite particles according to claim 2, characterized in that In the S1, the volume ratio of water glass to water is 1:(3-6); the resin is a cation exchange resin; and the substance added during the hydrolysis process is selected from one or more of formamide, N,N-dimethylformamide, hydrochloric acid, and nitric acid.
4. The pearlite particles according to claim 2, characterized in that In the S2, aging includes soaking the wet gel in an aging solution for 10-30 hours; the aging solution is selected from one of an ethanol aqueous solution and an ethanol-ethyl orthosilicate mixed solution; the replacement modification includes soaking the aged wet gel in a modifier for 10-30 hours; the modifier includes trimethylchlorosilane, n-heptane, and ethanol; and the drying is drying at normal pressure.
5. The pearlite particles according to claim 1, characterized in that The preparation method of the modified microcrystalline wax comprises the following steps: adding carbon nanotubes to the microcrystalline wax under temperature conditions T1, ultrasonic treatment, and heating and stirring evenly under temperature conditions T2 to obtain the modified microcrystalline wax.
6. The pearlite particles according to claim 5, characterized in that The T1 temperature is 85-95°C, the molecular weight of the microcrystalline wax is 500-700, and the mass ratio of the microcrystalline wax to the carbon nanotubes is 100:(0.1-0.5); the frequency of the ultrasonic treatment is 20-40kHz, the time of the ultrasonic treatment is 1-2h, the T2 temperature is 60-70°C, and the rotation speed is 50-200r / min.
7. A method for preparing the perlite particles according to any one of claims 1 to 6, characterized in that: The following steps are involved: S1, pretreating perlite to obtain pretreated perlite; S2, heating and mixing coconut oil, palmitic acid and modified microcrystalline wax to obtain a mixture; S3, mixing the pretreated perlite, the mixture and modified silica aerogel, and performing vacuum heating treatment to obtain the product.
8. The preparation method according to claim 7, characterized in that: In the above S1, the pretreatment includes adding water to the perlite, stirring, standing, and heating to obtain the perlite; the heating treatment includes first keeping the perlite at 100-110° C. for 1-2 hours, and then keeping the perlite at 200-300° C. for 5-20 minutes.
9. The preparation method according to claim 7, characterized in that: In the S2, the mass ratio of coconut oil, palmitic acid and modified microcrystalline wax is 14:(0.4-0.5):(0.8-1); The heating temperature is 70-95℃.
10. The preparation method according to claim 7, characterized in that: In the S3, the mass ratio of the mixture, the pretreated perlite and the modified silica aerogel is (0.1-2):1:(1-10); the vacuum heating treatment includes heating at 0.02-1Mpa and 60-80°C for 0.5-3h.