CN111334052A - Multifunctional antibacterial weather-resistant composite material composition and preparation method thereof - Google Patents
Multifunctional antibacterial weather-resistant composite material composition and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/44—Block-or graft-polymers containing polysiloxane sequences containing only polysiloxane sequences
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
- C08K3/013—Fillers, pigments or reinforcing additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The invention discloses a multifunctional antibacterial weather-resistant composite material composition and a preparation method thereof, belonging to the technical field of material compounding and being prepared from the following raw materials in parts by weight, 30-50 parts of end-capped multipurpose adjustable antibacterial organic silicon resin, 5-25 parts of calcium-based nano montmorillonite, 10-40 parts of pigment and filler, 0.1-0.5 part of dispersant, 20-30 parts of mixed solvent and 2-5 parts of alkaline solution. The resin provided by the invention has cations, has good surface activity and dispersibility, can disperse pigments and fillers well without adding a dispersant additive, and can ensure high composite performance, such as wear resistance, weather resistance, antibacterial property, sound absorption and the like by adopting the nano montmorillonite as a main functional filler; the hardness of the composite material is adjustable, and the composite material can be used in different occasions.
Description
Technical Field
The invention belongs to the technical field of material compounding, and particularly relates to a multifunctional antibacterial weather-resistant composite material composition and a preparation method thereof.
Background
The organic composite material is the result of the composite action of resin, functional filler, various assistants, curing agent and catalyst, and its main performance is determined greatly by the structure and physical and chemical properties of the resin. Resin modification is generally achieved by physical mixing techniques of different resins. The organic composite material has low cost, convenient raw material source and simple process, so the organic composite material is widely applied to the field of composite materials.
In recent years, a technique for obtaining a high-performance organic composite material by resin modification has been widely used. The organic composite material mainly comprises a base material, a functional filler, a dispersing agent, fibers, a mixed solvent, a curing agent, a catalyst and the like. The curing agent comprises: amine curing agents, isocyanate curing agents, and the like. Wherein most of the matrix materials are organic macromolecules, such as: phenolic resin, epoxy resin, amino resin, bismaleimide resin, unsaturated polyester resin matrix and the like, wherein the resin matrix belongs to organic polymers and has the characteristics of poor biodegradation property and heat resistance and aging resistance; the resin, the pigment, the filler and the inorganic fiber are poor in dispersibility and adhesive property, and can be well dispersed and soaked only by adding a plurality of additives, but the additives are dispersed and soaked to cause loss of mechanical property.
The prior art obtains high antibiotic, high strength, high resistant time combined material through looking for high antibiotic, multipurpose, high resistant time resin through the physics mixture, has certain effect, but still is far away not enough, especially is used for on needing better antibacterial property's combined material, and current resin can not reach the requirement, has the life-span simultaneously weak point that the later maintenance cost is high.
Disclosure of Invention
The invention aims to: aiming at the problems, the invention provides a multifunctional antibacterial weather-resistant composite material composition and a preparation method thereof.
The technical scheme adopted by the invention is as follows:
the multifunctional antibacterial weather-resistant composite material composition is prepared from the following raw materials, by weight, 30-50 parts of end-capped multipurpose adjustable antibacterial organic silicon resin, 5-25 parts of calcium-based nano montmorillonite, 10-40 parts of pigment and filler, 0.1-0.5 part of dispersing agent, 20-30 parts of mixed solvent and 2-5 parts of alkaline solution.
The dispersant of the present invention is preferably hammes 504S.
Preferably, the end-capped multipurpose adjustable antibacterial silicone resin is prepared from the following raw materials in parts by weight: 0-100 parts of siloxane flexible monomer, 0-100 parts of siloxane rigid monomer, 5-10 parts of aminosilane, 5-12 parts of alkylating agent W and 5-12 parts of quaternizing agent.
Preferably, the siloxane flexible monomer is any one or more of hexamethylcyclotrisiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane, decatetramethylcyclohexasiloxane, hexadecamethyloctasiloxane and dimethyldimethoxysilane; the rigid monomer is methyl phenyl dimethoxy silane or diphenyl dimethoxy silane; the aminosilane is
preferably, the mixed solvent is ethanol and isopropanol according to a mass ratio (0.8-1.2): 1 are mixed.
Preferably, the alkaline solution is 10-20% of KOH or NaOH aqueous solution in mass fraction.
Preferably, the particle size of the calcium-based nano montmorillonite is less than or equal to 100 nm; the pigment and filler is inorganic pigment and filler, and the particle size of the pigment and filler is less than or equal to 100 nm.
A preparation method of the multifunctional antibacterial weather-resistant composite material composition comprises the following steps:
s1, adding the mixed solvent into a dispersion container with a heat dissipation device, adding the dispersing agent and the alkaline solution, stirring and dispersing for 3-8min at the stirring speed of 200-400 r/min, then adding the end-capped multipurpose adjustable antibacterial organic silicon resin, stirring and dispersing for 8-14min at the stirring speed of 400-600 r/min, then grinding and dispersing, and then filtering and discharging to obtain the binder;
s2, distributing inorganic fiber by using the obtained binding material, adopting the pultrusion or mould pressing technology, pultrusion or mould pressing for 5-10min at the temperature of 160-170 ℃ to prepare a composite material product embryo, and then preserving heat for 4h in a drying room at the temperature of 120 ℃ to obtain the composite material composition product.
Preferably, the preparation of the end-capped multipurpose adjustable antibacterial silicone resin comprises the following steps:
s1-1, firstly, adding a siloxane flexible monomer, a siloxane rigid monomer, aminosilane and an alkaline solution into a reaction container, filling inert gas into a sealing device, starting heating, then heating to 80-86 ℃, reacting for 3-5 h until the viscosity reaches 1200-1400 mpa.s, adding acid to neutralize to the pH value of 6.8-7, and keeping the temperature of 80-86 ℃ for 1.5-3.5 h; distilling under reduced pressure to obtain low-boiling-point substances, namely the end-capped multipurpose silicon resin;
s1-2, cooling to 80-86 ℃, dropwise adding an alkylating agent W, refluxing for 2-2.5 h, dropwise adding a quaternizing agent, after dropwise adding, keeping the temperature of 80-86 ℃ for reflux reaction for 5-7h, and measuring the pH value, wherein the reaction end point is obtained when the pH value is 6-6.5;
and S1-3, distilling under reduced pressure to remove excessive quaternizing agent to obtain the thermosetting blocked multipurpose antibacterial organic silicon resin.
Preferably, the vacuum degree of the steps S1-1 and S1-2 is less than 20mmHg and the temperature is 102-105 ℃.
Preferably, the acid in step S1-1 is analytically pure formic acid or acetic acid.
Preferably, the grinding dispersion is carried out in the following manner: firstly, according to the following steps of zirconium beads: the weight ratio of the calcium-based nano montmorillonite to the pigment filler is (0.5-1.2): 1 adding zirconium beads, and grinding and dispersing for 0.5-1.5h at the rotating speed of 1000-.
The reaction principle of the invention is as follows: the following examples are given by taking dimethyldimethoxysilane as the siloxane soft monomer and methylphenyldimethoxysilane as the rigid monomer. (1) Dimethyl dimethoxy silane is a siloxane flexible monomer, methyl phenyl dimethoxy silane is a rigid monomer raw material, and amino silane is subjected to ring-opening reaction under an alkaline condition to generate hydroxyl silicone oil;
2) carrying out polycondensation reaction and end capping esterification on hydroxyl silicone oil and hydroxyl amino silicone oil to generate end capping multipurpose organic silicon resin;
(3) the blocked multipurpose organic silicon resin is subjected to the action of an alkylating agent and a quaternizing agent to generate the blocked multipurpose antibacterial organic silicon resin:
(4) the blocked multipurpose adjustable antibacterial organic silicon resin is subjected to hydrolytic polymerization under the action of strong alkali:
Compared with the prior art, the invention has the beneficial effects that:
(1) biodegradation resistance, heat resistance and aging resistance: the organic silicon has the characteristics of organic polymers and inorganic materials and has the characteristics of biodegradation resistance, heat resistance and aging resistance, and after the antibacterial bactericidal group is grafted on the main chain of the organic silicon, the biodegradation resistance, the heat resistance and the aging resistance of the organic silicon are obviously improved, and meanwhile, the local defects do not exist;
(2) the composite property is as follows: the resin provided by the invention has cations, has good surface activity and dispersibility, can disperse pigments and fillers well without adding a dispersing agent, and can ensure high composite performance, such as wear resistance, weather resistance, antibacterial property, sound absorption and the like by adopting the nano montmorillonite as a main functional filler;
(3) the hardness of the composite material is adjustable, and the composite material can be used for different occasions: because of excellent wear resistance, weather resistance, antibacterial property and sound absorption performance, the composite material can be used for prefabricated fiber composite materials and non-prefabricated composite materials, such as sports tracks and interior decoration (floors, facades, ceilings and the like), and meanwhile, the elasticity and hardness of the composite material can be adjusted.
Detailed Description
The present invention will be described in further detail in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the detailed description and specific examples, while indicating the preferred embodiment of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
A multifunctional antibacterial weather-resistant composite material composition comprises 35 parts of end-capped multipurpose adjustable antibacterial organic silicon resin, 25 parts of mixed solvent, 3 parts of alkaline solution, 10 parts of calcium-based nano montmorillonite, 27 parts of pigment and filler and 0.1 part of dispersing agent, wherein: end-capped multipurpose adjustable antibacterial silicone resin mixed solvent: the mass ratio of ethanol to isopropanol is 1: 1; alkaline solution: 10-20% of KOH or NaOH aqueous solution in mass fraction; calcium-based nano montmorillonite: the grain diameter is less than or equal to 100 nm; pigment and filler: the grain diameter is less than or equal to 100 nm; inorganic pigment and filler are adjusted according to color requirements, and the dispersant is as follows: haimines 504S.
The end-capped multipurpose adjustable antibacterial organic silicon resin is
Wherein a is 4; b is 1; c is 6; n is 1;m is 1.
The preparation process comprises the following steps:
weighing the mixed solvent, adding the mixed solvent into a dispersing container with a heat dissipation device, adding a dispersing agent and an alkaline solution, stirring and dispersing for 5min at a stirring speed of 300 revolutions/min, then adding the end-capped multipurpose adjustable antibacterial organic silicon resin, stirring and dispersing for 10min at a stirring speed of 500 revolutions/min, adding 3-5mm zirconium beads (mass ratio of zirconium beads: calcium-based nano-montmorillonite and pigment and filler is 0.8: 1), grinding and dispersing the calcium-based nano-montmorillonite and pigment and filler at a rotation speed of 1200 revolutions/min for 1h under heat dissipation, and filtering and discharging to obtain the binder. Then, the obtained binding material is used for distributing inorganic fibers, the process of pultrusion or mould pressing is adopted, the pultrusion or mould pressing is carried out for 5-10min at the temperature of 160-170 ℃, the composite material product embryo is prepared, and then the temperature is preserved for 4h in a drying room at the temperature of 120 ℃, and the composite material product is obtained.
Examples 2 to 6
Examples 2-6 the same as example 1 except that the contents of the respective components of the end-capped multi-purpose adjustable antibacterial silicone resin, the mixed solvent, the alkaline solution, the calcium-based nano-montmorillonite, the pigment and the dispersant were different.
TABLE 1 table of contents of components of examples 2 to 6
Examples 7 to 12
Examples 7-12 the procedure of example 1 was followed except that the multipurpose adjustable antimicrobial silicone resin used in the different hardness end caps was different from that used in example 1. Wherein the end-capped multipurpose adjustable antibacterial organic silicon resin is
Wherein a is 1-10; b is 1-2; c is 1 to 10; n is 1, 2 or 3; m is 1, 2 or 3.
Table 2 examples 7-12 specific values of a, b, c, n and m in the end-capped multipurpose adjustable antibacterial silicone resins
| Examples | a | b | c | n | m |
| 7 | 4 | 1 | 6 | 2 | 2 |
| 8 | 4 | 2 | 6 | 3 | 2 |
| 9 | 3 | 1 | 7 | 2 | 2 |
| 10 | 6 | 1 | 4 | 2 | 2 |
| 11 | 6 | 1 | 4 | 3 | 2 |
| 12 | 6 | 2 | 4 | 2 | 2 |
Experimental part
Description of the drawings: hardness (shore D) according to GB/T2411; tensile strength (MPa) tested according to GB/T13096-1; the antibacterial property is tested according to QB/T2591-2003; xenon lamp aging (with or without yellowing) was tested according to GB/T16422.2-2014/ISO 4892-2: 2006; ultraviolet lamp aging (with or without yellowing) is tested according to GB/T16422.3-2014/ISO 4892-3: 2006; the sound absorption coefficient is tested according to GB/T33620-2017(250 HZ).
Table 3 examples 1-12 performance test values
As can be seen from table 3, tests on the hardness, tensile strength, antibacterial property, xenon lamp aging (with or without yellowing), and ultraviolet lamp aging (with or without yellowing) of the multifunctional antibacterial weather-resistant composite material composition of the present invention show that after the antibacterial bactericidal group is grafted on the silicone main chain, the biodegradation resistance and heat and aging resistance of the composite material are significantly improved, and meanwhile, local defects do not exist, and the elasticity and hardness of the composite material are adjustable; the sound absorption coefficient measurement shows that the invention also has excellent sound absorption performance.
The above-mentioned embodiments only express the specific embodiments of the present application, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present application. It should be noted that, for those skilled in the art, without departing from the technical idea of the present application, several changes and modifications can be made, which are all within the protection scope of the present application.
Claims (10)
1. The multifunctional antibacterial weather-resistant composite material composition is characterized by being prepared from the following raw materials, by weight, 30-50 parts of end-capped multipurpose adjustable antibacterial organic silicon resin, 5-25 parts of calcium-based nano montmorillonite, 10-40 parts of pigment and filler, 0.1-0.5 part of dispersing agent, 20-30 parts of mixed solvent and 2-5 parts of alkaline solution.
2. The multifunctional antibacterial weather-resistant composite material composition as claimed in claim 1, wherein the end-capped multipurpose adjustable antibacterial silicone resin is prepared from the following raw materials in parts by weight: 0-100 parts of siloxane flexible monomer, 0-100 parts of siloxane rigid monomer, 5-10 parts of aminosilane, 5-12 parts of alkylating agent W and 5-12 parts of quaternizing agent.
3. The multifunctional antibacterial weather-resistant composite material composition as claimed in claim 2, wherein the siloxane flexible monomer is any one or more of hexamethylcyclotrisiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane, decatetramethylcyclohexasiloxane, hexadecylcyclooctasiloxane and dimethyldimethoxysilane; the rigid monomer is methyl phenyl dimethoxy silane or diphenyl dimethoxy silane; the aminosilane is
n is 1, 2 or 3; m is 1, 2 or 3; the quaternizing agent is benzyl halide or CH3CH2Cl; the alkylation reagent is methanol or a mixed reagent of ethanol and formaldehyde, and the molar ratio (0.8-1): 1.
4. the multifunctional antibacterial and weather-resistant composite material composition as claimed in claim 1, wherein the mixed solvent is ethanol and isopropanol in a mass ratio (0.8-1.2): 1 are mixed.
5. The multifunctional antibacterial and weatherable composite material composition as claimed in claim 1, wherein the alkaline solution is 10-20% by weight of KOH or NaOH aqueous solution.
6. The multifunctional antibacterial weather-resistant composite composition as claimed in claim 1, wherein the calcium-based nano montmorillonite has a particle size of 100nm or less; the pigment and filler is inorganic pigment and filler, and the particle size of the pigment and filler is less than or equal to 100 nm.
7. The preparation method of the multifunctional antibacterial weather-resistant composite material composition based on the claims 1 to 6 is characterized by comprising the following steps:
s1, adding the mixed solvent into a dispersion container with a heat dissipation device, adding the dispersing agent and the alkaline solution, stirring and dispersing for 3-8min at the stirring speed of 200-400 r/min, then adding the end-capped multipurpose adjustable antibacterial organic silicon resin, stirring and dispersing for 8-14min at the stirring speed of 400-600 r/min, then grinding and dispersing, and then filtering and discharging to obtain the binder;
s2, distributing inorganic fiber by using the obtained binding material, adopting the pultrusion or mould pressing technology, pultrusion or mould pressing for 5-10min at the temperature of 160-170 ℃ to prepare a composite material product embryo, and then preserving heat for 4h in a drying room at the temperature of 120 ℃ to obtain the composite material composition product.
8. The multifunctional antibacterial weatherable composite composition according to claim 7, wherein the preparation of the end-capped multipurpose adjustable antibacterial silicone resin comprises the following steps:
s1-1, firstly, adding a siloxane flexible monomer, a siloxane rigid monomer, aminosilane and an alkaline solution into a reaction container, filling inert gas into a sealing device, starting heating, then heating to 80-86 ℃, reacting for 3-5 h until the viscosity reaches 1200-1400 mpa.s, adding acid to neutralize to the pH value of 6.8-7, and keeping the temperature of 80-86 ℃ for 1.5-3.5 h; distilling under reduced pressure to obtain low-boiling-point substances, namely the end-capped multipurpose silicon resin;
s1-2, cooling to 80-86 ℃, dropwise adding an alkylating agent W, refluxing for 2-2.5 h, dropwise adding a quaternizing agent, after dropwise adding, keeping the temperature of 80-86 ℃ for reflux reaction for 5-7h, and measuring the pH value, wherein the reaction end point is obtained when the pH value is 6-6.5;
and S1-3, distilling under reduced pressure to remove excessive quaternizing agent to obtain the thermosetting blocked multipurpose antibacterial organic silicon resin.
9. The multifunctional antibacterial weather-resistant composite composition as claimed in claim 8, wherein the distillation conditions under reduced pressure of steps S1-1 and S1-2 are vacuum degree of less than 20mmHg and temperature of 102-105 ℃.
10. The preparation method of the multifunctional antibacterial weather-resistant composite material composition as claimed in claim 7, wherein the grinding dispersion method is as follows: firstly, according to the following steps of zirconium beads: the total weight ratio of the calcium-based nano montmorillonite to the pigment and filler is (0.5-1.2): 1 adding zirconium beads, and grinding and dispersing for 0.5-1.5h at the rotating speed of 1000-.
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| CN114409904A (en) * | 2022-01-19 | 2022-04-29 | 杭州一川新材料有限公司 | Preparation method and application of condensed type transparent silicone rubber |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114409904A (en) * | 2022-01-19 | 2022-04-29 | 杭州一川新材料有限公司 | Preparation method and application of condensed type transparent silicone rubber |
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