CN111925713A - Impact-resistant anti-static environment-friendly epoxy resin terrace and preparation method thereof - Google Patents
Impact-resistant anti-static environment-friendly epoxy resin terrace and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/04—Antistatic
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
Abstract
The invention belongs to the technical field of terraces, and particularly relates to an impact-resistant anti-static environment-friendly epoxy resin terrace and a preparation method thereof. The invention provides an anti-impact anti-static environment-friendly epoxy resin terrace which comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 60-90 parts of epoxy resin, 7.5-22 parts of color paste, 6-24 parts of fiber, 22-55 parts of resin colored sand and 3-8 parts of diluent; the component B comprises: 55-85 parts of a curing agent. Through selecting modified bamboo pulp fiber for use, the flexural strength, compressive strength, impact resistance and the like of the epoxy resin terrace are improved, and the problems of heavy object crushing and the like in the use process of the actual ground of some factories can be solved. The epoxy resin terrace is environment-friendly and accords with the environmental protection concept.
Description
Technical Field
The invention belongs to the technical field of terraces, and particularly relates to an impact-resistant anti-static environment-friendly epoxy resin terrace and a preparation method thereof.
Background
With the progress of science and technology, the terrace industry in China has a leap development, and the terrace industry is widely applied to a plurality of specific fields, such as plastic tracks of playgrounds, repairing of building concrete cracks, filling and repairing of leaks between beam-building points, indoor floor decoration and the like.
To date, the development of terrace materials has been mature, and is mainly divided into three major resin systems, namely epoxy resin, acrylic resin and polyurethane resin. In these systems, the matrix resin is generally an amorphous viscous liquid which has no distinct melting point, is easily softened by heating, gradually melts and becomes sticky, and is insoluble in water. By adding a proper amount of curing agent or initiator into the matrix resin, the resin can have physical and mechanical properties which can be practically used after being cured, and can be widely applied to actual life and production. According to different specific requirements, a plurality of other components, such as cement, mortar, a plasticizer and other materials, can be added into the matrix resin, so that the specific performance of one aspect of the matrix resin is further enhanced, the application of the matrix resin is more targeted and purposeful, and the greater economic value of the matrix resin is improved.
The terrace is also suitable for the ground decoration of some factories at present, especially for companies needing to transport materials frequently under the daily condition, especially for electronic factories and the like, and higher requirements are provided for the antistatic property and the impact resistance of the terrace, while the antistatic property and the impact resistance of the terrace which is commonly used at present are relatively lower, so that the demands of the enterprises in the future cannot be met. Therefore, the development of the anti-impact anti-static environment-friendly epoxy resin terrace has practical application value.
Disclosure of Invention
In order to solve the technical problems, the invention provides an anti-impact anti-static environment-friendly epoxy resin terrace, which comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 60-90 parts of epoxy resin, 7.5-22 parts of color paste, 6-24 parts of fiber, 22-55 parts of resin colored sand and 3-8 parts of diluent; the component B comprises: 55-85 parts of a curing agent.
In a preferred embodiment, the epoxy resin is at least one selected from the group consisting of a bisphenol a type epoxy resin, a polyimide-modified bisphenol a type epoxy resin, a polyglycidyl ether type epoxy resin, a glycidyl ester type epoxy resin, a bisphenol F type epoxy resin, a biphenol type epoxy resin, and a novolac polyepoxy resin.
As a preferable technical solution, the epoxy resin is a polyimide modified bisphenol a epoxy resin.
As a preferable technical scheme, the fiber is selected from at least one of wood pulp fiber, bamboo pulp fiber and surface pulp fiber.
As a preferred technical scheme, the fiber is C15-C22 olefine acid modified fiber.
In a preferred embodiment, the C15-C22 olefinic acid is at least one selected from the group consisting of 39912oleic acid, oleic acid, octadecenoic acid, nonadeca-5, 8,11, 14-tetraenoic acid, 10-nonadecenoic acid, 13-docosenoic acid, eicosa-5, 7,9,14, 17-pentaenoic acid, erucic acid and eleostearic acid.
As a preferred technical solution, the resin colored sand includes resin colored sand and epoxy resin colored sand containing modified graphene oxide.
As a preferable technical scheme, the weight ratio of the resin colored sand to the epoxy resin colored sand containing the modified graphene oxide is 3-5: 1.
as a preferable technical scheme, the component A raw material also comprises 7-15 parts of filler, 1-3 parts of defoaming agent and 0.1-1.5 parts of flatting agent;
the invention provides a preparation method of the impact-resistant anti-static environment-friendly epoxy resin terrace, which comprises the following steps:
the method comprises the following steps: adding a diluent and color paste into the epoxy resin, and stirring for 10-15 minutes at a stirring speed of 300-400 rpm to obtain a mixed solution 1;
step two: adding resin color sand and fiber into the mixed solution 1, stirring at the stirring speed of 700-;
step three: and (4) mixing the mixture obtained in the step two with a curing agent of the component B to obtain the impact-resistant anti-static environment-friendly epoxy resin terrace.
Has the advantages that: through selecting modified bamboo pulp fiber for use, the flexural strength, compressive strength, impact resistance and the like of the epoxy resin terrace are improved, and the problems of heavy object crushing and the like in the use process of the actual ground of some factories can be solved. The epoxy resin terrace is environment-friendly and accords with the environmental protection concept.
Detailed Description
For purposes of the following detailed description, it is to be understood that the invention may assume various alternative variations and step sequences, except where expressly specified to the contrary.
In order to solve the problems, the invention provides an anti-impact anti-static environment-friendly epoxy resin terrace which comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 60-90 parts of epoxy resin, 7.5-22 parts of color paste, 6-24 parts of fiber, 22-55 parts of resin colored sand and 3-8 parts of diluent; the component B comprises: 55-85 parts of a curing agent.
In a preferred embodiment, the epoxy resin is at least one selected from the group consisting of a bisphenol a type epoxy resin, a polyimide-modified bisphenol a type epoxy resin, a polyglycidyl ether type epoxy resin, a glycidyl ester type epoxy resin, a bisphenol F type epoxy resin, a biphenol type epoxy resin, and a novolac polyepoxy resin.
In a preferred embodiment, the epoxy resin is a polyimide modified bisphenol a type epoxy resin.
In a preferred embodiment, the epoxy resin is a polyimide modified bisphenol a type epoxy resin and a phenol formaldehyde epoxy resin. The weight ratio of the polyimide modified bisphenol A epoxy resin to the phenol formaldehyde epoxy resin is 10-15: 1. the phenol formaldehyde epoxy resin is purchased from the Jinan Yisheng resin Co., Ltd, and has the model of F-44.
The preparation method of the polyimide modified bisphenol A epoxy resin comprises the following steps:
(1) 2.13g of 2, 4-dihydroxy m-phenylenediamine hydrochloride and 1mL of triethylamine are dissolved in 25mL of N-methylpyrrolidone, 3.1g of diphenyl ether tetracarboxylic dianhydride, 10mL of toluene and 1.0g of glacial acetic acid are added, then the temperature is increased to 180 ℃, the temperature is kept for 5 hours, after the reaction is finished, the mixture is precipitated in methanol, filtered and dried in vacuum, and the polyimide containing hydroxyl is obtained.
(2) Mixing the following components in parts by weight of 100: 40: 90: and (2) mixing the bisphenol A type epoxy resin of 1, the polyimide obtained in the step (1), nadic anhydride and 2, 4, 6-tris (dimethylaminomethyl) phenol, heating while stirring uniformly, heating at the temperature of 120 ℃ for 1h, and then continuously heating to the temperature of 150 ℃ for 3h to obtain the epoxy resin.
The fiber is selected from at least one of wood pulp fiber, bamboo pulp fiber and surface pulp fiber; preferably, the fiber is a C15-C22 olefine acid modified fiber.
The preparation method of the C15-C22 olefine acid modified fiber comprises the following steps:
s1, reacting C15-C22 olefine acid with thionyl chloride at 50-70 ℃ for 10-14h, and distilling under reduced pressure to remove excessive thionyl chloride to prepare C15-C22 olefine acid chloride, wherein the molar ratio of C15-C22 olefine acid to thionyl chloride is 1: 1.1;
s2, drying the fibers, adding the fibers into a universal pulverizer to perform thorough pulverization, wherein the pulverized fineness range is 20-120 meshes;
s3, adding 2g of the fiber treated in the step S2, 0.5-1g C15-C22 gadoleic acid acyl chloride and 0.02g of 4-dimethylamino pyridine into 70mL of anhydrous pyridine, reacting at 60 ℃ for 2h, adding 30-40mL of ethanol, continuing to react for 30min, filtering and drying to obtain the cellulose fiber.
More preferably, the fiber is C15-C22 olefine acid modified bamboo pulp fiber. The bamboo pulp fiber is prepared by pulping bamboo chips, then preparing pulp from the pulp, and then spinning the pulp by a wet method.
The C15-C22 olefine acid is selected from at least one of 39912andoleic acid, oleic acid, octadecenoic acid, nonadeca-5, 8,11, 14-tetraenoic acid, 10-nonadecenoic acid, 13-docosenoic acid, eicosa-5, 7,9,14, 17-pentaenoic acid, erucic acid and eleostearic acid.
The resin color sand comprises resin color sand and epoxy resin color sand containing modified graphene oxide; the weight ratio of the resin color sand to the epoxy resin color sand containing the modified graphene oxide is 3-5: 1.
the preparation method of the epoxy resin colored sand containing the modified graphene oxide comprises the following steps:
1. graphene oxide preparation
(1): adding 1.0g of graphite and 0.2g of sodium nitrate into a flask weighed with 23.0mL of concentrated sulfuric acid, stirring for 30 minutes, cooling the bottom of the flask to below zero by adopting an ice bath, adding 3.00g of potassium permanganate, continuously stirring until the mixture is uniformly mixed, removing the ice bath, heating to 35 ℃, keeping for 30 minutes, continuously heating to 70 ℃, keeping for 30 minutes, and then adding three times of deionized water, 3mL each time, and 5 minutes each time. Then adding 40mL of water to stop the reaction, naturally cooling the reaction to room temperature, and adding 10mL of 30 wt% hydrogen peroxide;
(1-2): adding deionized water, naturally settling, removing supernatant, washing for three times, collecting sample by filtering, and drying to obtain graphite oxide precursor;
(1-3): roasting the graphite oxide precursor obtained in the step (1-2): under the protection of inert gas, heating to 500 ℃, the heating rate is 50 ℃ per minute, keeping the temperature for 1 hour, and taking out a roasted sample after cooling to room temperature;
(1-4): adding the roasted sample and 0.2g of sodium nitrate into a flask weighed with 23.0mL of concentrated sulfuric acid, stirring for 30 minutes, cooling the bottom of the flask to below zero by adopting an ice bath, then adding 3.00g of potassium permanganate, continuously stirring until the mixture is uniformly mixed, removing the ice bath, then heating to 35 ℃, keeping for 30 minutes, continuously heating to 70 ℃, keeping for 30 minutes, then adding three times of deionized water, 3mL each time, and 5 minutes each time. Then adding 40mL of water to stop the reaction, naturally cooling the reaction to room temperature, and adding 10mL of 30 wt% hydrogen peroxide;
(1-5): adding deionized water, naturally settling, removing supernatant, repeatedly washing for three times, collecting samples in a filtering mode, and drying to obtain the graphene oxide.
2. Preparing modified graphene oxide: and (3) dispersing the graphene oxide prepared in the step (1) in 500mL of deionized water to prepare a graphene oxide colloidal suspension. Adding 5mL of concentrated sulfuric acid into the suspension, heating the reactor to 110 ℃, adding 5mL of malonic acid into the reactor, reacting for 4min to obtain a modified graphene oxide dispersion solution, and carrying out vacuum filtration, washing and drying on the modified graphene oxide dispersion solution to obtain modified graphene oxide;
3. preparing epoxy resin sand containing modified graphene oxide: adding 30g of the modified graphene oxide obtained in the step into 50g of bisphenol A epoxy resin, adding 3g of allyl glycidyl ether and 1g of defoamer polyoxyethylene polyoxypropylene pentaerythritol ether, mechanically stirring with 400-.
In a preferred embodiment, the epoxy resin sand containing modified graphene oxide has an average particle size of 0.1 to 0.6 mm.
The diluent is a monoepoxy glycidyl ether reactive diluent and/or a diepoxy glycidyl ether reactive diluent.
The synthetic method of the diluent comprises the following steps:
(1) in a four-necked flask equipped with a reflux condenser, an isobaric dropping funnel, a stirrer and a thermometer, 8.81g of 1, 4-butenediol, 8.42g of KOH solid, 0.40g of tetrabutylammonium bromide and 100mL of a solution having a volume ratio of 2: 1, uniformly stirring the mixed solution of toluene and water;
(2) 18.50g of epichlorohydrin is slowly dropped at 40 ℃ and reacted for 6 hours. And (3) removing the organic solvent by rotary evaporation, washing the obtained aqueous solution with 50mL of cyclohexane, extracting with dichloromethane, and removing the solvent by evaporation to obtain the compound.
In a preferred embodiment, the component A raw material also comprises 7-15 parts of filler, 1-3 parts of defoaming agent and 0.1-1.5 parts of leveling agent;
the defoaming agent is not particularly limited, and is a defoaming agent commonly used in the art, and alcohols defoaming agent, ether defoaming agent, silicone modified polyether defoaming agent; in the present application, the defoaming agent is polyoxyethylene polyoxypropylene pentaerythritol ether.
The filler is at least one selected from silicon powder, alumina, silicon dioxide, calcium carbonate, silicon carbide and mica powder. In the present application, the filler is silica.
The color paste is used for adjusting the color of the epoxy resin coating, and is not particularly limited.
The leveling agent is not particularly limited and is a leveling agent commonly used in the art, and in the present application, the leveling agent is BYK-333.
The curing agent is an acid anhydride curing agent and aromatic polyamine; the curing agent is selected from at least one of 4,4' -diaminodiphenylmethane, maleic anhydride, phthalic anhydride, tetrahydrophthalic anhydride, polyazelaic anhydride, polysebacic anhydride, diphenyl ether tetracarboxylic dianhydride, 2, N-dimethyl-N- (3, 3-diphenylpropyl) -1-amino-2-propanol, ethyl 2- ((1S,2R) -2-hydroxy-1, 2-diphenylethylamino) acetate, 4' -diamino-3, 3' -dichlorodiphenylmethane, 4' -diaminodiphenyl ether and 4,4' -diaminodiphenylmethane. The curing agent in this application is 4,4' -diaminodiphenylmethane.
The second aspect of the invention provides a preparation method of the epoxy resin terrace, which comprises the following steps:
the method comprises the following steps: adding a diluent and color paste into the epoxy resin, and stirring for 10-15 minutes at a stirring speed of 300-400 rpm to obtain a mixed solution 1;
step two: adding resin color sand and fiber into the mixed solution 1, stirring at the stirring speed of 700-;
step three: and (4) mixing the mixture obtained in the step two with a curing agent of the component B to obtain the impact-resistant anti-static environment-friendly epoxy resin terrace.
Preferably, the preparation method of the epoxy resin terrace comprises the following steps:
the method comprises the following steps: sequentially adding a defoaming agent, a flatting agent, color paste and a diluent into the epoxy resin, and stirring for 10-15 minutes at a stirring speed of 300-400 rpm to obtain a mixed solution 1;
step two: adding a filler into the mixed solution 1, and stirring for 30-40 minutes at a stirring speed of 600-700 rpm to obtain a mixed solution 2;
step three: adding resin color sand and fiber into the mixed solution 2, stirring at the stirring speed of 700-;
step four: and (4) mixing the mixture obtained in the step three with a curing agent of the component B to obtain the impact-resistant anti-static environment-friendly epoxy resin terrace.
The toughness of the epoxy resin terrace is improved by introducing the fibers; the fiber is polymerized by a plurality of D-glucosyl groups, contains more polar groups and has poor compatibility with the epoxy resin, and the compatibility of the fiber and the epoxy resin is improved and the impact resistance of the epoxy resin terrace is improved by the C15-C22 gadoleic acid acyl chloride modified fiber; particularly, when the C15-C22 gadoleic acid acyl chloride is eleostearic acid acyl chloride and the fiber is bamboo pulp fiber, the compressive strength of the obtained epoxy resin terrace is over 50MPa, and the impact resistance is improved to about 6J, so that the problems of heavy object crushing and the like in the actual ground use process of some factories can be well solved; and the defects that the bamboo pulp fiber is easy to absorb water, the floor is not flat due to shrinkage and the like are overcome, the water absorption rate of the epoxy resin floor is reduced, and the appearance is smooth.
The present invention will be specifically described below by way of examples. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention.
In addition, the starting materials used are all commercially available, unless otherwise specified.
Examples
Example 1
The utility model provides an anti-static environment-friendly epoxy terrace that shocks resistance, includes A component and B component, by weight, A component includes following raw materials: 90 parts of epoxy resin, 22 parts of color paste, 24 parts of fiber, 55 parts of resin color sand, 8 parts of diluent, 15 parts of filler silicon dioxide, 3 parts of defoamer polyoxyethylene polyoxypropylene pentaerythritol ether and 3 parts of flatting agent BYK-3331.5; the component B comprises: 85 parts of curing agent 4,4' -diaminodiphenylmethane.
The epoxy resin is polyimide modified bisphenol A epoxy resin.
The preparation method of the polyimide modified bisphenol A epoxy resin comprises the following steps:
(1) 2.13g of 2, 4-dihydroxy m-phenylenediamine hydrochloride and 1mL of triethylamine are dissolved in 25mL of N-methylpyrrolidone, 3.1g of diphenyl ether tetracarboxylic dianhydride, 10mL of toluene and 1.0g of glacial acetic acid are added, then the temperature is increased to 180 ℃, the temperature is kept for 5 hours, after the reaction is finished, the mixture is precipitated in methanol, filtered and dried in vacuum, and the polyimide containing hydroxyl is obtained.
(2) Mixing the following components in parts by weight of 100: 40: 90: and (2) mixing the bisphenol A type epoxy resin of 1, the polyimide obtained in the step (1), nadic anhydride and 2, 4, 6-tris (dimethylaminomethyl) phenol, heating while stirring uniformly, heating at the temperature of 120 ℃ for 1h, and then continuously heating to the temperature of 150 ℃ for 3h to obtain the epoxy resin.
The trade names of 2, 4, 6-tris (dimethylaminomethyl) phenol are DMP-30, K-54.
The fiber is eleostearic acid modified bamboo pulp fiber (eleostearic acid: CAS No. 506-23-0), and the bamboo pulp fiber is purchased from Jim Jiu Miao textile Co.
The preparation method of the eleostearic acid modified fiber comprises the following steps:
s1, reacting eleostearic acid with thionyl chloride at 60 ℃ for 12 hours, and distilling under reduced pressure to remove excessive thionyl chloride to prepare eleostearic acid acyl chloride, wherein the molar ratio of eleostearic acid to thionyl chloride is 1: 1.1;
s2, drying the fibers, adding the fibers into a universal pulverizer to perform thorough pulverization, wherein the pulverized fineness range is 100-120 meshes;
s3, adding 2g of the fiber treated in the step S2, 0.6g of eleostearic acid acyl chloride and 0.02g of 4-dimethylamino pyridine into 70mL of anhydrous pyridine, reacting at 60 ℃ for 2h, adding 40mL of ethanol, continuing to react for 30min, filtering and drying to obtain the fiber.
The resin color sand comprises resin color sand and epoxy resin color sand containing modified graphene oxide; the weight ratio of the resin color sand to the epoxy resin color sand containing the modified graphene oxide is 4: 1. the mesh number of the resin color sand is 80 meshes, and the purchasing company is a Wanyu mineral product company Limited.
The preparation method of the epoxy resin colored sand containing the modified graphene oxide comprises the following steps:
1. graphene oxide preparation
(1): adding 1.0g of graphite and 0.2g of sodium nitrate into a flask weighed with 23.0mL of concentrated sulfuric acid, stirring for 30 minutes, cooling the bottom of the flask to below zero by adopting an ice bath, adding 3.00g of potassium permanganate, continuously stirring until the mixture is uniformly mixed, removing the ice bath, heating to 35 ℃, keeping for 30 minutes, continuously heating to 70 ℃, keeping for 30 minutes, and then adding three times of deionized water, 3mL each time, and 5 minutes each time. Then adding 40mL of water to stop the reaction, naturally cooling the reaction to room temperature, and adding 10mL of 30 wt% hydrogen peroxide;
(1-2): adding deionized water, naturally settling, removing supernatant, washing for three times, collecting sample by filtering, and drying to obtain graphite oxide precursor;
(1-3): roasting the graphite oxide precursor obtained in the step (1-2): under the protection of inert gas, heating to 500 ℃, the heating rate is 50 ℃ per minute, keeping the temperature for 1 hour, and taking out a roasted sample after cooling to room temperature;
(1-4): adding the roasted sample and 0.2g of sodium nitrate into a flask weighed with 23.0mL of concentrated sulfuric acid, stirring for 30 minutes, cooling the bottom of the flask to below zero by adopting an ice bath, then adding 3.00g of potassium permanganate, continuously stirring until the mixture is uniformly mixed, removing the ice bath, then heating to 35 ℃, keeping for 30 minutes, continuously heating to 70 ℃, keeping for 30 minutes, then adding three times of deionized water, 3mL each time, and 5 minutes each time. Then adding 40mL of water to stop the reaction, naturally cooling the reaction to room temperature, and adding 10mL of 30 wt% hydrogen peroxide;
(1-5): adding deionized water, naturally settling, removing supernatant, repeatedly washing for three times, collecting samples in a filtering mode, and drying to obtain the graphene oxide.
2. Preparing modified graphene oxide: and (3) dispersing the graphene oxide prepared in the step (1) in 500mL of deionized water to prepare a graphene oxide colloidal suspension. Adding 5mL of concentrated sulfuric acid into the suspension, heating the reactor to 110 ℃, adding 5mL of malonic acid into the reactor, reacting for 4min to obtain a modified graphene oxide dispersion solution, and carrying out vacuum filtration, washing and drying on the modified graphene oxide dispersion solution to obtain modified graphene oxide;
3. preparing epoxy resin sand containing modified graphene oxide: adding 30g of the modified graphene oxide obtained in the step into 50g of bisphenol A epoxy resin, adding 3g of allyl glycidyl ether and 1g of defoamer polyoxyethylene polyoxypropylene pentaerythritol ether, mechanically stirring with 400-.
The average particle size of the epoxy resin sand containing the modified graphene oxide is 0.5 mm.
The synthetic method of the diluent comprises the following steps:
(1) in a four-necked flask equipped with a reflux condenser, an isobaric dropping funnel, a stirrer and a thermometer, 8.81g of 1, 4-butenediol, 8.42g of KOH solid, 0.40g of tetrabutylammonium bromide and 100mL of a solution having a volume ratio of 2: 1, uniformly stirring the mixed solution of toluene and water;
(2) 18.50g of epichlorohydrin is slowly dropped at 40 ℃ and reacted for 6 hours. And (3) removing the organic solvent by rotary evaporation, washing the obtained aqueous solution with 50mL of cyclohexane, extracting with dichloromethane, and removing the solvent by evaporation to obtain the compound.
The preparation method of the epoxy resin terrace comprises the following steps:
the method comprises the following steps: adding a defoaming agent, a flatting agent, color paste and a diluent into the epoxy resin in sequence, and stirring at a stirring speed of 400 revolutions per minute for 10 minutes to obtain a mixed solution 1;
step two: adding a filler into the mixed solution 1, and stirring for 40 minutes at a stirring speed of 600 revolutions per minute to obtain a mixed solution 2;
step three: adding the resin colored sand and the fibers into the mixed solution 2, stirring for 30 minutes at the stirring speed of 900 revolutions per minute, grinding and sieving;
step four: and (4) mixing the mixture obtained in the step three with a curing agent of the component B to obtain the impact-resistant anti-static environment-friendly epoxy resin terrace.
Example 2
The utility model provides an anti static environment-friendly epoxy terrace is prevented to shock, embodiment is with embodiment 1, and the difference lies in, including A component and B component, by weight, A component includes following raw materials: 60 parts of epoxy resin, 7.5 parts of color paste, 6 parts of fiber, 22 parts of resin colored sand, 3 parts of diluent, 7 parts of filler silicon dioxide, 1 part of defoaming agent polyoxyethylene polyoxypropylene pentaerythritol ether and 1 part of flatting agent BYK-3330.1; the component B comprises: 55 parts of curing agent 4,4' -diaminodiphenylmethane.
Example 3
The utility model provides an anti static environment-friendly epoxy terrace is prevented to shock, embodiment is with embodiment 1, and the difference lies in, including A component and B component, by weight, A component includes following raw materials: 70 parts of epoxy resin, 15 parts of color paste, 15 parts of fiber, 30 parts of resin colored sand, 5 parts of diluent, 12 parts of filler silicon dioxide, 2 parts of defoamer polyoxyethylene polyoxypropylene pentaerythritol ether and BYK-3331.0 parts of flatting agent; the component B comprises: 70 parts of curing agent 4,4' -diaminodiphenylmethane.
Example 4
The specific implementation mode of the impact-resistant anti-static environment-friendly epoxy resin terrace is the same as that in embodiment 3, and the difference is that 0 part of fiber is adopted.
Example 5
The specific implementation mode of the impact-resistant anti-static environment-friendly epoxy resin terrace is the same as that in embodiment 3, and the difference is that the fiber is bamboo pulp fiber.
Example 6
The impact-resistant anti-static environment-friendly epoxy resin floor is the same as that in embodiment 3, and is different from the embodiment in that 36 parts of fibers are adopted
Example 7
The specific implementation mode of the impact-resistant anti-static environment-friendly epoxy resin floor is the same as that of example 3, and the difference is that the eleostearic acid modified bamboo pulp fiber is replaced by decatetraenoic acid modified bamboo pulp fiber, and the CAS number of the decatetraenoic acid is 17016-39-6.
Example 8
The specific implementation mode of the impact-resistant anti-static environment-friendly epoxy resin terrace is the same as that in example 3, and the difference is that the eleostearic acid modified bamboo pulp fiber is replaced by methyldioctadecyl-5, 9-dienoic acid modified bamboo pulp fiber, and the CAS number of the methyldioctadecyl-5, 9-dienoic acid is 153081-63-1.
Example 9
The specific implementation mode of the impact-resistant anti-static environment-friendly epoxy resin terrace is the same as that in example 3, and the difference is that the epoxy resin is polyimide modified bisphenol A epoxy resin and phenol formaldehyde epoxy resin. The weight ratio of the polyimide modified bisphenol A epoxy resin to the phenol formaldehyde epoxy resin is 12: 1. the phenol formaldehyde epoxy resin is purchased from the Jinan Yisheng resin Co., Ltd, and has the model of F-44.
Example 10
The specific implementation mode of the impact-resistant anti-static environment-friendly epoxy resin terrace is the same as that in example 3, and the difference is that the weight part of the epoxy resin color sand containing the modified graphene oxide is 0.
Performance testing
Surface resistance: standard range of 5X 104-1×106。
Appearance, impact resistance, breaking strength, compressive strength, elongation at break test: reference is made to GB/T22374-2008 floor materials. The results are shown in Table 1.
TABLE 1
Through selecting modified bamboo pulp fiber for use, the flexural strength, compressive strength, impact resistance and the like of the epoxy resin terrace are improved, and the problems of heavy object crushing and the like in the use process of the actual ground of some factories can be solved. Besides the same performance as that of the epoxy resin terraces obtained in examples 1-3, the epoxy resin terraces obtained when the epoxy resin is polyimide-modified bisphenol A epoxy resin and phenol formaldehyde epoxy resin have lower water absorption than the terraces obtained when the epoxy resin is polyimide-modified bisphenol A epoxy resin, and the water absorption is less than 0.01%, so that the molecular regularity of the terraces is presumed to be improved by the specific epoxy resin.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in other forms, and any person skilled in the art may modify or change the technical content of the above disclosure into equivalent embodiments with equivalent changes, but all those simple modifications, equivalent changes and modifications made to the above embodiments according to the technical spirit of the present invention still belong to the protection scope of the present invention.
Claims (10)
1. The utility model provides an anti-static environment-friendly epoxy terrace that shocks resistance which comprises a component and a component B, by weight, the component A includes following raw materials: 60-90 parts of epoxy resin, 7.5-22 parts of color paste, 6-24 parts of fiber, 22-55 parts of resin colored sand and 3-8 parts of diluent; the component B comprises: 55-85 parts of a curing agent.
2. The impact-resistant antistatic environment-friendly epoxy resin terrace as claimed in claim 1, wherein the epoxy resin is selected from at least one of bisphenol A type epoxy resin, polyimide modified bisphenol A type epoxy resin, polyglycidyl ether type epoxy resin, glycidyl ester type epoxy resin, bisphenol F type epoxy resin, biphenol type epoxy resin, and novolac polyepoxy resin.
3. The impact-resistant antistatic environment-friendly epoxy resin terrace as claimed in claim 2, wherein the epoxy resin is a polyimide modified bisphenol A epoxy resin.
4. The impact-resistant antistatic environment-friendly epoxy resin floor as claimed in claim 1, wherein the fiber is selected from at least one of wood pulp fiber, bamboo pulp fiber and surface pulp fiber.
5. The impact-resistant antistatic environment-friendly epoxy resin floor as claimed in claim 4, wherein the fiber is C15-C22 olefine acid modified fiber.
6. The impact-resistant antistatic environment-friendly epoxy resin terrace as claimed in claim 5, wherein the C15-C22 olefine acid is selected from the group consisting of 39912oleic acid, oleic acid, octadecenoic acid, nonadeca-5, 8,11, 14-tetraenoic acid, 10-nonadecenoic acid, 13-docosenoic acid, eicosa-5, 7,9,14, 17-pentaenoic acid, erucic acid and eleostearic acid.
7. The impact-resistant antistatic environment-friendly epoxy resin terrace as claimed in claim 1, wherein the resin color sand comprises resin color sand and epoxy resin color sand containing modified graphene oxide.
8. The impact-resistant antistatic environment-friendly epoxy resin terrace as claimed in claim 7, wherein the weight ratio of the resin color sand to the epoxy resin color sand containing modified graphene oxide is 3-5: 1.
9. the impact-resistant antistatic environment-friendly epoxy resin terrace as claimed in claim 1, wherein the component A further comprises 7-15 parts of filler, 1-3 parts of defoaming agent and 0.1-1.5 parts of leveling agent.
10. The preparation method of the impact-resistant antistatic environment-friendly epoxy resin floor as claimed in any one of claims 1 to 8, characterized by comprising the following steps:
the method comprises the following steps: adding a diluent and color paste into the epoxy resin, and stirring for 10-15 minutes at a stirring speed of 300-400 rpm to obtain a mixed solution 1;
step two: adding resin color sand and fiber into the mixed solution 1, stirring at the stirring speed of 700-;
step three: and (4) mixing the mixture obtained in the step two with a curing agent of the component B to obtain the impact-resistant anti-static environment-friendly epoxy resin terrace.
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| JPH09296321A (en) * | 1996-05-07 | 1997-11-18 | Kohjin Co Ltd | Production of rayon fiber containing docosahexaenoic acid |
| CN102643439A (en) * | 2012-05-09 | 2012-08-22 | 中国林业科学研究院林产化学工业研究所 | Manufacture method of eleostearic acid graft modification wood fibers |
| CN104745047A (en) * | 2015-04-22 | 2015-07-01 | 广东耐迪化工有限公司 | Self-leveling sand color terrace material as well as preparation method and construction method thereof |
| CN109593440A (en) * | 2018-12-17 | 2019-04-09 | 浙江润奥环保科技有限公司 | A kind of environment-friendly type nano graphene floor material and preparation method thereof |
| CN110819205A (en) * | 2019-11-11 | 2020-02-21 | 温州奥源新材料科技有限公司 | Graphene composite impact-resistant anti-static environment-friendly coating material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH09296321A (en) * | 1996-05-07 | 1997-11-18 | Kohjin Co Ltd | Production of rayon fiber containing docosahexaenoic acid |
| CN102643439A (en) * | 2012-05-09 | 2012-08-22 | 中国林业科学研究院林产化学工业研究所 | Manufacture method of eleostearic acid graft modification wood fibers |
| CN104745047A (en) * | 2015-04-22 | 2015-07-01 | 广东耐迪化工有限公司 | Self-leveling sand color terrace material as well as preparation method and construction method thereof |
| CN109593440A (en) * | 2018-12-17 | 2019-04-09 | 浙江润奥环保科技有限公司 | A kind of environment-friendly type nano graphene floor material and preparation method thereof |
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