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CN-122012015-A - Deodone oxime type matte organic silicon sealant and preparation method thereof

CN122012015ACN 122012015 ACN122012015 ACN 122012015ACN-122012015-A

Abstract

The invention discloses a ketoxime-removing type matte organic silicon sealant and a preparation method thereof, and relates to the technical field of sealants. The raw materials of the organic silicon sealant comprise alpha, omega-dihydroxypolydimethylsiloxane, dimethyl silicone oil, fumed silica, modified nano calcium carbonate, barium sulfate, a composite cross-linking agent, dibutyl tin dilaurate, heptanoic acid, silane coupling agent mixed solution, diphenyl dimethoxy silane, an antioxidant and a defoaming agent, and the raw materials of the composite cross-linking agent comprise methyl tributyl ketoxime silane, methyl tri (methyl isobutyl ketoxime) silane, deionized water and acetic acid. The preparation method of the organic silicon sealant comprises the steps of functional component pre-preparation, basic filler dispersion, addition of a cross-linking agent and an auxiliary agent, and preparation of the organic silicon sealant. The organic silicon sealant prepared by the invention has stable matte effect, excellent mechanical property and storage stability.

Inventors

  • MA JIAN
  • LI KAI
  • Xia changcheng
  • Lang Linlin
  • FU YOUKUN
  • ZHANG QIANG
  • CHEN SHUHAI

Assignees

  • 山东景茂新材料有限公司

Dates

Publication Date
20260512
Application Date
20260414

Claims (9)

  1. 1. The preparation method of the deone oxime type matte organic silicon sealant is characterized by comprising the steps of functional component pre-preparation, basic filler dispersion, addition of a cross-linking agent and an auxiliary agent, and preparation of the organic silicon sealant; The preparation method comprises the steps of mixing methyl tributyl ketoxime silane and methyl tri (methyl isobutyl ketoxime) silane under the protection of nitrogen, stirring uniformly, dropwise adding deionized water and acetic acid, carrying out heat preservation reaction, and then carrying out vacuum dehydration to obtain a composite cross-linking agent; The base filler is dispersed, namely alpha, omega-dihydroxyl polydimethylsiloxane and simethicone are uniformly stirred, then fumed silica is added, the temperature is raised, the stirring kettle is vacuumized and stirred, then the temperature is lowered, and modified nano calcium carbonate and barium sulfate are added and stirred; the cross-linking agent and the auxiliary agent are added, namely, the vacuum state of a stirring kettle is kept, the temperature is naturally reduced, the composite cross-linking agent, the silane coupling agent mixed solution, the diphenyl dimethoxy silane, the antioxidant and the defoaming agent are sequentially added into the stirring kettle, and the stirring is carried out; The preparation method of the organic silicon sealant comprises the steps of maintaining the vacuum state of a stirring kettle, maintaining the temperature of the stirring kettle, adding dibutyltin dilaurate, stirring, adding heptanoic acid, continuing stirring, and filtering by a filter screen to obtain the organic silicon sealant.
  2. 2. The preparation method of the deodone oxime type matte organosilicon sealant is characterized by comprising, by weight, 55-85 parts of alpha, omega-dihydroxy polydimethylsiloxane, 10-30 parts of simethicone, 10-20 parts of fumed silica, 80-120 parts of modified nano calcium carbonate, 2-5 parts of barium sulfate, 5-12 parts of a compound cross-linking agent, 0.3-0.8 part of dibutyltin dilaurate, 0.1-0.3 part of heptanoic acid, 1.5-4.5 parts of a silane coupling agent mixed solution, 0.3-1 part of diphenyl dimethoxy silane, 0.1-0.5 part of an antioxidant and 0.1-0.3 part of a defoaming agent.
  3. 3. The preparation method of the deodone oxime type matte organosilicon sealant according to claim 1 is characterized in that the mass ratio of the methyltributylketon oxime silane to the methyltributylketon oxime silane is (6-7) to (3-4).
  4. 4. The method for preparing the deodone oxime type matte organosilicon sealant according to claim 1, wherein the dosage of deionized water in the step of preparing the functional component is 1-1.5% of the total mass of methyltributylketon oxime silane and methyltributylketon oxime silane.
  5. 5. The method for preparing the deodone oxime type matte organosilicon sealant according to claim 1, wherein in the step of preparing the functional component, the consumption of acetic acid is 0.05-0.15% of the total mass of methyltributylketon oxime silane and methyltributylketon oxime silane.
  6. 6. The preparation method of the deodone oxime type matte organic silicon sealant according to claim 1 is characterized in that in the preparation step of the functional component, the functional component is dehydrated in vacuum, the temperature is 80-90 ℃, the vacuum degree is-0.095 MPa to-0.098 MPa, and the dehydration time is 1-2h.
  7. 7. The preparation method of the ketoxime type matte organosilicon sealant is characterized in that the zinc stearate accounts for 1.5-2% of the mass of the nano calcium carbonate.
  8. 8. The preparation method of the deodone oxime type matte organosilicon sealant according to claim 1 is characterized in that the mass ratio of the silane coupling agent KH-560 to the silane coupling agent KH-792 is (1.8-2): 1.
  9. 9. The method for preparing the deodone oxime type matte organic silicon sealant according to claim 1, which is characterized by comprising the following steps: and in the step of dispersing the basic filler, the stirring kettle is vacuumized, wherein the vacuum degree is between-0.095 MPa and-0.098 MPa.

Description

Deodone oxime type matte organic silicon sealant and preparation method thereof Technical Field The invention relates to the technical field of sealants, in particular to a deodone oxime type matte organic silicon sealant and a preparation method thereof. Background The ketoxime-removed organosilicon sealant can be cured without illumination at room temperature, has excellent weather resistance and good bonding performance to various base materials, and is widely applied to the fields of building decoration, automobile manufacturing, electronic element packaging and the like. However, with the continuous expansion and high-end application of the application scene, the market puts more severe requirements on the comprehensive performance of the sealant, and the traditional formula and technology expose a plurality of limitations to be solved urgently. In the existing product, single ketoxime cross-linking agents such as methyl tributyl ketoxime silane and the like are commonly adopted in the industry, and the cross-linking reaction activity and the rate of the single ketoxime cross-linking agents are difficult to accurately regulate and control, so that the stability of the matte effect is not only influenced, but also the problems of high viscosity, slow solidification and the like of the sealant after long-term storage are easily caused, and the shelf life and the use reliability of the product are severely restricted. The prior art with publication number CN118931481A discloses a high-performance matte silicone sealant and a preparation method thereof, and the prior art is mainly a dealcoholization type system, has low curing speed in a low-temperature environment and has insufficient storage stability. The prior art with the publication number of CN119684962A discloses a long-storage-period double-component silicone sealant and a preparation method thereof, and the prior art can realize the long-term storage aim, but is a double-component system, has insufficient construction convenience and lacks the design of a matte effect. In summary, the prior art solutions, although improving certain properties of silicone sealants to some extent, still have the technical problem of failing to combine stable matte effect, excellent mechanical properties and excellent storage stability. Disclosure of Invention In order to solve the problems in the prior art, the invention provides a ketoxime-removing type matte organic silicon sealant and a preparation method thereof, and the aim of preparing the organic silicon sealant with stable matte effect, good mechanical property and excellent storage stability is fulfilled. In order to achieve the above purpose, the following technical scheme is adopted: a preparation method of a deone oxime type matte organic silicon sealant comprises the steps of functional component preparation, basic filler dispersion, addition of a cross-linking agent and an auxiliary agent, and preparation of the organic silicon sealant; The raw materials are, by weight, 55-85 parts of alpha, omega-dihydroxy polydimethylsiloxane, 10-30 parts of simethicone, 10-20 parts of fumed silica, 80-120 parts of modified nano calcium carbonate, 2-5 parts of barium sulfate, 5-12 parts of a compound cross-linking agent, 0.3-0.8 part of dibutyltin dilaurate, 0.1-0.3 part of heptanoic acid, 1.5-4.5 parts of a silane coupling agent mixed solution, 0.3-1 part of diphenyl dimethoxy silane, 0.1-0.5 part of an antioxidant and 0.1-0.3 part of a defoaming agent. The viscosity of the alpha, omega-dihydroxy polydimethylsiloxane at 25 ℃ is 50000-100000 mPa.s. The particle size of the fumed silica is 12-20nm. The defoaming agent is an organic silicon defoaming agent, and BYK-066N is selected. The antioxidant is hindered phenol antioxidant, and Irganox1010 is selected. The functional component is prepared by mixing methyl tributyl ketoxime silane and methyl tri (methyl isobutyl ketoxime) silane under the protection of nitrogen, stirring uniformly, dropwise adding deionized water and acetic acid, carrying out heat preservation reaction, then carrying out vacuum dehydration to obtain a composite cross-linking agent, mixing nano calcium carbonate and zinc stearate uniformly, heating and stirring to obtain modified nano calcium carbonate, and mixing silane coupling agent KH-560 and silane coupling agent KH-792 uniformly to obtain a silane coupling agent mixed solution. Further, the mass ratio of the methyltributylketonoxime silane to the methyltributylketonoxime silane is (6-7) (3-4). The dosage of the deionized water is 1 to 1.5 percent of the total mass of the methyltributylketon oxime silane and the methyltributylketon oxime silane. The dosage of the acetic acid is 0.05-0.15% of the total mass of the methyltributylketonoxime silane and the methyltributylketonoxime silane. The vacuum dehydration is carried out at 80-90 ℃ and a vacuum degree of-0.095 MPa to-0.098 MPa for 1-2h. Further, the dosage of the zinc stearate is 1.5-2% of t