CN112573839B - Anti-aggregation treatment method for inorganic fibers and anti-aggregation inorganic fibers prepared by same - Google Patents
Anti-aggregation treatment method for inorganic fibers and anti-aggregation inorganic fibers prepared by same Download PDFInfo
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- CN112573839B CN112573839B CN202011403067.1A CN202011403067A CN112573839B CN 112573839 B CN112573839 B CN 112573839B CN 202011403067 A CN202011403067 A CN 202011403067A CN 112573839 B CN112573839 B CN 112573839B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/10—Coating
- C03C25/12—General methods of coating; Devices therefor
- C03C25/16—Dipping
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/10—Coating
- C03C25/24—Coatings containing organic materials
- C03C25/40—Organo-silicon compounds
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/10—Coating
- C03C25/465—Coatings containing composite materials
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- General Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
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- Polymerisation Methods In General (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
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Abstract
The invention discloses an inorganic fiber anti-aggregation treatment method and an anti-aggregation inorganic fiber prepared by the method, wherein the method comprises the following steps: a) Dispersing: placing inorganic fibers and a dispersing agent in an organic solvent at the temperature of 0-30 ℃ and stirring until the inorganic fibers and the dispersing agent are fully dispersed; b) Coupling: adding acryloxy silane and hydrolysis catalyst, and stirring for 0.1-5 hr; c) Polymerization: then adding initiator, heating to 40-80 deg.C, continuously stirring for 0.1-5 hr so as to obtain the invented anti-agglomeration inorganic fibre. The invention has the following advantages: the formed low-surface-energy protective layer is stable, strong in environmental tolerance, low in raw material cost and simple in treatment process. The prepared inorganic fiber has very good anti-agglomeration effect, can be stood for 10 days at room temperature without agglomeration, and has wide engineering application prospect in different coating formula fields.
Description
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to an inorganic fiber anti-aggregation treatment method and anti-aggregation inorganic fibers prepared by the same.
Background
In the fields of construction, aviation, aerospace and energy, the demand for high-temperature resistant paint is large. In these high temperature resistant coatings, inorganic fibers are an important high temperature resistant aid. The inorganic fiber is a chemical fiber prepared by taking mineral substances as raw materials and melting the mineral substances at a high temperature in proportion. Common varieties are: glass, silica, asbestos, alumina, zirconia, mullite, basalt, ceramic, and the like. The inorganic fiber generally has the excellent performances of high dimensional stability, low heat conductivity coefficient, good electrical insulation, good sound absorption performance, high filtering efficiency and the like.
In the coating application process of inorganic fibers, the dispersion performance of the inorganic fibers in water is a key factor affecting the overall performance of the formulation. Because the surface of the inorganic fiber contains a large amount of Si-OH and Al-OH, hydrogen bonds with strong acting force are generated between the inorganic fiber and the inorganic fiber, and the fiber is longer and flexible, spontaneous aggregation and even winding agglomeration can occur among the fibers, so that the inorganic fiber is difficult to disperse. The inorganic fiber sample is directly immersed in water to generate uneven dispersion, and even under the condition of high-shear stirring, only a small part of fibers can be dispersed into single fibers.
Zhang Sufeng et al [ Chinese paper making, 2013 (08): 37-40 ] using different organic solvents, breaking the molecular forces between glass fibers, making them susceptible to dissociation into individual fiber dispersion states. However, the chemical state of the surface of the glass fiber is not changed compared with that of the glass fiber before the treatment, and the dispersibility of the glass fiber is easily affected by adding other auxiliary agents into the formula.
Hu Fuzeng et al [ composite theory, 1989,6 (1): 7-13 ] studied the influence of silane coupling agents on the surface properties of glass fibers, and found that the silane coupling agents can significantly reduce the surface free energy and polarity of glass fibers and improve the dispersion stability thereof.
CN103570255 provides a glass fiber sizing composition comprising carbon nanomaterial, dispersant, polymer emulsion, coupling agent and solvent, which sizing composition forms a coating on the surface of the fiber by means of the polymer emulsion film-forming agent and the coupling agent together to improve the compatibility and bridging effect of the fiber and matrix resin and promote the deposition of the carbon nanomaterial on the surface of the fiber. The method has the advantages of high raw material cost, complex process and difficult industrial popularization.
Disclosure of Invention
The invention aims at overcoming the defects in the prior art and provides an inorganic fiber anti-aggregation treatment method and an anti-aggregation inorganic fiber prepared by the method.
The invention aims at realizing the following technical scheme:
the invention provides an inorganic fiber anti-aggregation treatment method, which comprises the following steps:
a) Dispersing: placing inorganic fibers and a dispersing agent in an organic solvent at the temperature of 0-30 ℃ and stirring until the inorganic fibers and the dispersing agent are fully dispersed;
b) Coupling: adding acryloxy silane and hydrolysis catalyst, and stirring for 0.1-5 hr;
c) Polymerization: adding initiator, heating to 40-80 deg.c, stirring for 0.1-5 hr to obtain inorganic fiber; in the polymerization step, the polymerization rate is too low, the polymerization rate is too high, and the explosion polymerization is easy to occur.
Preferably, the inorganic fiber is made of one or more of glass, silicon dioxide, asbestos, aluminum oxide, zirconium oxide, mullite, basalt and ceramic; the diameter of the inorganic fiber is 3-50 mu m, and the short cutting length is 0.1-50 mm.
Preferably, the dispersing agent is one or more of alkylphenol ethoxylates, fatty alcohol ethoxylates, fatty acid polyoxyethylene esters, polyoxyethylene alkylamines, polyoxyethylene alkylamides, polyvinylpyrrolidone, polyethylene glycol, polyvinyl alcohol and polyoxyethylene polyoxypropylene block copolymers.
Preferably, the organic solvent is one or more of ethanol, methanol, acetone, ethyl acetate, methyl ethyl ketone, methyl isobutyl ketone, tetrahydrofuran, toluene, xylene, N-dimethylformamide and dichloromethane.
Preferably, the acryloxy silane is one or more of 3- (acryloxy) propyl triethoxy silane, 3- (acryloxy) propyl trimethoxy silane, 3- (methacryloxy) propyl triethoxy silane, 3- (methacryloxy) propyl trimethoxy silane, vinyl trimethoxy silane and vinyl triethoxy silane.
Preferably, the hydrolysis catalyst is one or more of sulfuric acid, hydrochloric acid, nitric acid and ammonia water; the mass percentage of the hydrolysis catalyst is 0.1-30%.
Preferably, the initiator is one or more of azodiisobutyronitrile, azodiisoheptonitrile, benzoyl peroxide, lauroyl peroxide, hydrogen peroxide, cumene hydroperoxide, potassium persulfate and ammonium persulfate.
Preferably, the inorganic fiber, the dispersant, the organic solvent, the acryloyloxy silane, the hydrolysis catalyst and the initiator are respectively 1 part, 0.01-0.5 part, 10-500 parts, 0.1-1 part and 0.01-1 part by mass;
the rotation speed of each stirring is 2000-15000 rpm; the stirring may be assisted simultaneously with ultrasound.
The invention also provides an anti-agglomeration inorganic fiber which comprises the following components in parts by mass:
1 part of inorganic fiber, 0.01 to 0.5 part of dispersing agent, 10 to 500 parts of organic solvent, 0.1 to 1 part of acryloyloxy silane, 0.1 to 1 part of hydrolysis catalyst and 0.01 to 1 part of initiator.
Preferably, the inorganic fiber is made of one or more of glass, silicon dioxide, asbestos, aluminum oxide, zirconium oxide, mullite, basalt and ceramic; the diameter of the inorganic fiber is 3-50 mu m, and the short cutting length is 0.1-50 mm;
the dispersing agent is one or more of alkylphenol ethoxylates, fatty alcohol ethoxylates, fatty acid polyoxyethylene esters, polyoxyethylene alkylamines, polyoxyethylene alkylamides, polyvinylpyrrolidone, polyethylene glycol, polyvinyl alcohol and polyoxyethylene polyoxypropylene block copolymers;
the organic solvent is one or more of ethanol, methanol, acetone, ethyl acetate, methyl ethyl ketone, methyl isobutyl ketone, tetrahydrofuran, toluene, xylene, N-dimethylformamide and dichloromethane;
the acryloyloxy silane is one or more of 3- (acryloyloxy) propyl triethoxysilane, 3- (acryloyloxy) propyl trimethoxysilane, 3- (methacryloyloxy) propyl triethoxysilane, 3- (methacryloyloxy) propyl trimethoxysilane, vinyl trimethoxysilane and vinyl triethoxysilane;
the hydrolysis catalyst is one or more of sulfuric acid, hydrochloric acid, nitric acid and ammonia water; the mass percentage of the hydrolysis catalyst is 0.1-30%;
the initiator is one or more of azodiisobutyronitrile, azodiisoheptonitrile, benzoyl peroxide, lauroyl peroxide, hydrogen peroxide, cumene hydroperoxide, potassium persulfate and ammonium persulfate.
Preferably, the anti-agglomeration inorganic fiber can be stored for standby after filtration.
The acryloyloxy silane disclosed by the invention can play a role of a coupling agent, and can be used for converting the hydroxyl with stronger polarity on the surface of the original inorganic fiber into the ether bond with weaker polarity, so that the surface energy is reduced, and the aggregation trend of the fiber is reduced; on the other hand, the molecular structure of the acryloyloxy silane is provided with polymerizable double bonds, and polymerization reaction is generated under the initiation action of an initiator and a certain temperature, so that a relatively dense and stable low-surface-energy protective layer is formed, and the anti-aggregation capability of the inorganic fiber is enhanced.
Compared with the prior art, the invention has the following beneficial effects:
1. the low surface energy protective layer formed by the anti-agglomeration treatment method of the inorganic fiber is stable, has strong environmental tolerance, low raw material cost and simple treatment process.
2. The inorganic fiber prepared by the invention has very good anti-agglomeration effect, and can be kept stand for 10 days at room temperature without agglomeration.
3. The anti-agglomeration inorganic fiber prepared by the invention has wide engineering application prospect in the field of different paint formulas.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the present invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications could be made by those skilled in the art without departing from the inventive concept. These are all within the scope of the present invention.
Example 1
A glass fiber anti-agglomeration treatment method comprises the following steps:
a) Dispersing: 1 g of glass fiber (diameter: 10 μm, short cut length: 2 mm) and 0.1 g of alkylphenol ethoxylate dispersant (OP-10) were placed in 200 g of ethanol at 20℃and stirred at 8000rpm until they were sufficiently dispersed;
b) Coupling: 0.2 g of 3- (acryloyloxy) propyltriethoxysilane and 0.5 g of sulfuric acid in water (15%) were added and stirring was continued at 8000rpm for 1hr;
c) Polymerization: then 0.02 g of azodiisobutyronitrile initiator is added, the temperature is raised to 60 ℃, and stirring is continued for 1hr at 8000rpm, so as to obtain the anti-agglomeration glass fiber. No agglomeration phenomenon is seen when the mixture is stood for 10 days at room temperature.
Example 2
The asbestos fiber agglomeration preventing treatment process includes the following steps:
a) Dispersing: 1 g of asbestos fiber (diameter 3 μm, short cut length 0.1 mm) and 0.01 g of polyvinylpyrrolidone dispersing agent were placed in 10 g of acetone at 0℃and stirred at 2000rpm until fully dispersed;
b) Coupling: 0.1 g of 3- (acryloyloxy) propyltrimethoxysilane and 0.1 g of aqueous sulfuric acid (0.1%) were added and stirring was continued at 2000rpm for 5hr;
c) Polymerization: then 0.01 g of benzoyl peroxide initiator is added, the temperature is raised to 40 ℃, and stirring is continued for 5 hours at 2000rpm, thus obtaining the anti-agglomeration asbestos fiber. No agglomeration phenomenon is seen when the mixture is stood for 10 days at room temperature.
Example 3
An alumina fiber anti-agglomeration treatment method comprises the following steps:
a) Dispersing: 1 g of alumina fiber (diameter 50 μm, short cut length 50 mm) and 0.5 g of polyethylene glycol dispersant were placed in 500 g of toluene at 30℃and stirred at 15000rpm until they were sufficiently dispersed;
b) Coupling: 1 g of 3- (methacryloyloxy) propyltriethoxysilane and 1 g of aqueous sulfuric acid (30%) were added and stirring was continued at 15000rpm for 0.1hr;
c) Polymerization: then 0.1 g of cumene hydroperoxide initiator is added, the temperature is raised to 80 ℃, and stirring is continued for 0.1hr at 15000rpm, thus obtaining the anti-agglomeration alumina fiber. No agglomeration phenomenon is seen when the mixture is stood for 10 days at room temperature.
Example 4
A mullite fiber anti-agglomeration treatment method comprises the following steps:
a) Dispersing: at 25 ℃,1 gram of mullite fiber (diameter of 10 μm, short cut length of 3 mm) and 0.3 gram of polyoxyethylene polyoxypropylene block copolymer (PEO-PPE) dispersant are placed in 100 grams of ethyl acetate, and stirred at 10000rpm under the assistance of ultrasonic waves until the mixture is fully dispersed;
b) Coupling: 0.3 g of 3- (methacryloyloxy) propyltrimethoxysilane and 0.8 g of aqueous ammonia (8%) were added and stirring was continued for 2hr at 10000 rpm;
c) Polymerization: and adding 0.05 g of ammonium persulfate initiator, heating to 50 ℃, and continuously stirring at 10000rpm for 2 hours to obtain the anti-agglomeration mullite fiber. No agglomeration phenomenon is seen when the mixture is stood for 10 days at room temperature.
Example 5
The basalt fiber anti-agglomeration treatment method comprises the following steps:
a) Dispersing: 1 g basalt fiber (diameter 12 μm, short cut length 6 mm) and 0.2 g polyoxyethylene polyoxypropylene block copolymer (PEO-PPE) dispersant were placed in 50 g N, N-dimethylformamide at 15℃and stirred at 5000rpm until fully dispersed;
b) Coupling: 0.3 g of 3- (methacryloyloxy) propyltrimethoxysilane and 0.7 g of sulfuric acid solution (8%) were added and stirring was continued at 5000rpm for 2hr;
c) Polymerization: and adding 0.05 g of lauroyl peroxide initiator, heating to 70 ℃, and continuously stirring at 5000rpm for 2hr to obtain the anti-agglomeration basalt fiber. No agglomeration phenomenon is seen when the mixture is stood for 10 days at room temperature. Filtering, storing for 10 days, and dispersing according to the condition of a), wherein no agglomeration phenomenon is found.
Comparative example 1
A method for preparing a glass fiber dispersion system, comprising the following steps:
a) Dispersing: 1 g of glass fiber (diameter: 10 μm, short cut length: 2 mm) and 0.1 g of alkylphenol ethoxylate dispersant (OP-10) were placed in 200 g of ethanol at 20℃and stirred at 8000rpm until they were sufficiently dispersed;
b) Coupling: 0.2 g of 3- (acryloyloxy) propyltriethoxysilane and 0.5 g of sulfuric acid in water (15%) were added, and stirring was continued at 8000rpm for 1hr.
The obtained glass fiber dispersion system stands for 1 day at room temperature to see obvious agglomeration phenomenon.
Comparative example 2
A process for preparing a glass fiber dispersion, which differs from the process of example 1 only in that: in step b) of this comparative example, 3- (acryloyloxy) propyltriethoxysilane was not added.
The obtained glass fiber dispersion system stands for 1 day at room temperature to see obvious agglomeration phenomenon.
Comparative example 3
A process for preparing a glass fiber dispersion, which differs from the process of example 1 only in that: in step b) of this comparative example, no aqueous sulfuric acid solution was added.
The obtained glass fiber dispersion system stands for 2 days at room temperature to obtain obvious agglomeration phenomenon.
Comparative example 4
A process for preparing a glass fiber dispersion, which differs from the process of example 1 only in that: in step b) of this comparative example gamma-aminopropyl triethoxysilane was used instead of 3- (acryloyloxy) propyl triethoxysilane.
The obtained glass fiber dispersion system stands for 5 days at room temperature to obtain obvious agglomeration phenomenon.
There are many ways in which the invention may be practiced, and what has been described above is merely a preferred embodiment of the invention. It should be noted that the above examples are only for illustrating the present invention and are not intended to limit the scope of the present invention. It will be apparent to those skilled in the art that modifications may be made without departing from the principles of the invention, and such modifications are intended to be within the scope of the invention.
Claims (5)
1. The anti-agglomeration treatment method for the inorganic fibers is characterized by comprising the following steps of:
a) Dispersing: placing inorganic fibers and a dispersing agent in an organic solvent at the temperature of 0-30 ℃ and stirring until the inorganic fibers and the dispersing agent are fully dispersed;
b) Coupling: adding acryloyloxy silane and a hydrolysis catalyst, and continuously stirring for 0.1-5 hr;
c) Polymerization: then adding an initiator, heating to 40-80 ℃, and continuously stirring for 0.1-5 hr to obtain the anti-agglomeration inorganic fiber;
the acryloyloxy silane is one or more of 3- (acryloyloxy) propyl triethoxysilane, 3- (acryloyloxy) propyl trimethoxysilane, 3- (methacryloyloxy) propyl triethoxysilane, 3- (methacryloyloxy) propyl trimethoxysilane, vinyl trimethoxysilane and vinyl triethoxysilane;
the hydrolysis catalyst is one or more of sulfuric acid, hydrochloric acid, nitric acid and ammonia water; the mass percentage of the hydrolysis catalyst is 0.1-30%;
the initiator is one or more of azodiisobutyronitrile, azodiisoheptonitrile, benzoyl peroxide, lauroyl peroxide, hydrogen peroxide, cumene hydroperoxide, potassium persulfate and ammonium persulfate;
the dispersing agent is one or more of alkylphenol ethoxylates, fatty alcohol ethoxylates, fatty acid polyoxyethylene esters, polyoxyethylene alkylamines, polyoxyethylene alkylamides, polyvinylpyrrolidone, polyethylene glycol, polyvinyl alcohol and polyoxyethylene polyoxypropylene block copolymers;
the inorganic fiber, the dispersing agent, the organic solvent, the acryloyloxy silane, the hydrolysis catalyst and the initiator are respectively 1 part, 0.01-0.5 part, 10-500 parts, 0.1-1 part and 0.01-1 part by mass.
2. The method for preventing agglomeration of inorganic fibers according to claim 1, wherein the inorganic fibers are made of one or more of glass, silica, asbestos, alumina, zirconia, mullite, basalt and ceramic; the diameter of the inorganic fiber is 3-50 mu m, and the short cut length is 0.1-50 mm.
3. The method for anti-aggregation treatment of inorganic fibers according to claim 1, wherein the organic solvent is one or more of ethanol, methanol, acetone, ethyl acetate, methyl ethyl ketone, methyl isobutyl ketone, tetrahydrofuran, toluene, xylene, N-dimethylformamide and methylene chloride.
4. The method for anti-aggregation treatment according to claim 1, wherein the rotation speed of each of the stirring is 2000 to 15000rpm; the stirring is simultaneously assisted by ultrasound.
5. An anti-aggregation inorganic fiber, wherein the anti-aggregation inorganic fiber is prepared by the anti-aggregation treatment method of the inorganic fiber according to any one of claims 1 to 4.
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| CN101708963B (en) * | 2009-08-07 | 2012-12-05 | 甘肃紫鑫矿业煤化工有限公司 | Andalusite fiber size and preparation method thereof |
| CN103570255B (en) * | 2012-08-07 | 2016-08-10 | 重庆国际复合材料有限公司 | A kind of glass fiber infiltration agent composition, preparation method and application |
| CN104446075B (en) * | 2014-11-28 | 2017-09-29 | 长安大学 | A kind of basalt chopped fiber dispersant and its application process |
| CN105271830B (en) * | 2015-10-20 | 2018-08-21 | 江门市新会区美亚化工有限公司 | A kind of basalt continuous fiber sizing agent special of nano modification and preparation method thereof |
| CN107640913B (en) * | 2017-08-22 | 2019-10-01 | 江苏大学 | A kind of preparation method and applications of Basalt fiber surface modification coating |
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