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Reaction resin comprising core-shell particles and method for the production thereof and the use thereof

A reactive, resinous technology used in the field of thermosetting plastics to solve problems such as material defects, large solvent consumption, and complexity

Inactive Publication Date: 2010-03-24
WACKER CHEM GMBH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of the described method is that the amount of solvent used is sometimes very large, which in turn requires a very complicated way of removing it, and if it is not removed completely, the result may be defects in the material during hardening of the reactive resin
Another disadvantage is the use of inorganic salts which, even after extraction, can still be found in the organic solution of the siloxane particles, since they absorb water to a certain extent, with the result that traces of aqueous salts are always present, therefore Entrainment of salt-containing contaminants in reactive resins, which is undesirable for reactive resins in electronic applications

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] Embodiment 1 (not the present invention):

[0065] Production of graft base:

[0066] 3800 g of water and 19 g (1.9 wt%, based on the Si compound) of dodecylbenzenesulfonic acid were heated to 85°C. Add 855g (2.9mol, 74mol%) octamethylcyclotetrasiloxane, 97g (0.7mol, 18mol%) methyltrimethoxysilane and 66g (0.3mol, 8mol%) methacryloxypropyltrimethyl Oxysilane mixture and continued stirring at 85°C for 4 hours. After removal of about 400 g of distillate, the product obtained was a dispersion with a solids content of 21% by weight and a particle size of 111 nm.

[0067] graft:

[0068] 13050 g of the dispersion were inertized with nitrogen in a 15 L reactor and the pH was adjusted to 4. Add 90g methyl methacrylate, by adding 5.2g (0.6wt%, based on monomer) K 2 S 2 o 8 and 18 g (2.1 wt%, based on monomer) NaHSO 3 (37 wt% aqueous solution) initiated the polymerization. Within 1 hour, a further 780 g of methyl methacrylate were added, and the mixture was heated to 65...

Embodiment 2

[0069] Embodiment 2 (of the present invention):

[0070] Production of graft base:

[0071] 3000 g of water, 5 g (0.5 wt%, based on the Si compound) of dodecylbenzenesulfonic acid and 8 g of acetic acid were heated to 90°C. A mixture of 855 g (92 mol %) of octamethylcyclotetrasiloxane and 95 g (5 mol %) of vinyltrimethoxysiloxane was added within 2 hours and stirring was continued for 3 hours.

[0072] Grafting of Shell B:

[0073] Then 63 g (2 mol %) of methacryloxypropyltrimethoxysilane were added, and stirring was continued at 90° C. for 1 hour. This gave a dispersion with a solids content of 23 wt% and an average particle size of 122 nm.

[0074] Grafting of Shell D:

[0075] 13050 g of the dispersion were inertized with nitrogen in a 25 L reactor and the pH was adjusted to 4. Add 90g methyl methacrylate, by adding 5.2g (0.6wt%, based on monomer) K 2 S 2 o 8 and 18 g (2.1 wt%, based on monomer) NaHSO 3 (37 wt% aqueous solution) initiated the polymerization. Withi...

Embodiment 3

[0076] Embodiment 3 (of the present invention):

[0077] Production of graft base:

[0078] 3000 g of water, 5 g (0.5 wt%, based on the Si compound) of dodecylbenzenesulfonic acid and 8 g of acetic acid were heated to 90°C. A mixture of 855 g (92 mol %) of octamethylcyclotetrasiloxane and 95 g (5 mol %) of vinyltrimethoxysiloxane was added within 2 hours and stirring was continued for 3 hours.

[0079] Grafting of Shell B:

[0080] Then 63 g (2 mol %) of methacryloxypropyltrimethoxysilane were added, and stirring was continued at 90° C. for 1 hour. This gave a dispersion with a solids content of 23% by weight and an average particle size of 132 nm.

[0081] Grafting of Shell D:

[0082] 13050 g of the dispersion were inertized with nitrogen in a 25 L reactor and the pH was adjusted to 4. Add 90g methyl methacrylate, by adding 5.2g (0.6wt%, based on monomer) K 2 S 2 o 8 and 18 g (2.1 wt%, based on monomer) NaHSO 3 (37 wt% aqueous solution) initiated the polymerization....

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Abstract

The invention relates to a composition comprising (A) 50 - 99.5 weight % of a reaction resin or a reaction resin mixture that can be processed into a thermosetting material and is liquid at temperatures in the range from 15 to 100 DEG C and has an average molecular weight of 200 to 500,000, and having a sufficient number of suitable reactive groups for the curing process, and (B) 0.5 to 50 weight% of one or more three-dimensionally cross-linked redispersed polyorganosiloxane rubbers, which are homogenously present in the reaction resin or reaction resin mixture in a finely distributed form aspolyorganosiloxane rubber particles having a diameter of 0.001 to 0.4 [mu]m, the polyorganosiloxane rubber particles being made of a core (a) made of a silicone-organic polymer and an organopolymer shell (d) and optionally two inner shells (b) and (c), the inner shell (c) being an organic polymer and the inner shell (b) being a silicone-organic polymer, comprising (a) 20 to 95 weight %, relativeto the total weight of the polyorganosiloxane rubber particle, of a core polymer of the general formula (R3SiO1 / 2)w(R2SiO2 / 2)x.(RSiO3 / 2)y.(SiO4 / 2)z, wherein w = 0 to 20 Mol %, x = 80 to 99.5 Mol%, y =0.5 to 10 Mol%, z = 0 to 10 Mol%, (b) 0 to 40 weight %, relative to the total weight of the polyorganosiloxane rubber particle, of a polydialkylsiloxane shell made of units of the formula (R3SiO1 / 2)w(R2SiO2 / 2) x.(RSiO3 / 2) y.(SiO4 / 2)z, wherein w = 0 to 20 Mol %, x = 0 to 99.5 Mol%, y = 0.5 to 100 Mol%, z = 0 to 50 Mol%, (c) 0 to 40 weight %, relative to the total weight of the polyorganosiloxane rubber particle, of a shell made of organopolymer monoolefinically or polyolefinically unsaturated monomers, and (d) 5 to 95 weight %, relative to the total weight of the polyorganosiloxane rubber particle, of a shell made of organopolymer monoolefinically unsaturated monomers, wherein R means identical or different monovalent alkyl or alkenyl radicals having 1 to 6 carbon atoms, aryl radicals, orsubstituted hydrocarbon radicals.

Description

technical field [0001] The present invention relates to reactive resins comprising core-shell particles, methods for their production, and their use in the production of thermoset plastics with improved mechanical properties such as fracture toughness and impact resistance. Background technique [0002] The crosslink density of crosslinking reactive resins is usually very high, which gives them some valuable properties and makes them the most widely used polymers outside of thermoplastics. Among these properties are hardness, strength, chemical resistance and resistance to variable temperatures. This makes the reactive resins suitable for use in many fields, for example for the production of fiber-reinforced plastics, for insulating materials in electrical engineering, and for the production of construction adhesives, high-pressure laminates, baking varnishes, etc. [0003] Thermosets also have a serious drawback that often prevents their application. Due to their highly c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L51/08C08F283/12
CPCC08L51/08C08L51/04C08L51/085C08F283/12C08L2666/02
Inventor O·舍费尔H·奥斯瓦德鲍尔
Owner WACKER CHEM GMBH
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