CN113565290A - High-thermal-stability SPC (modified polyvinyl chloride) floor and manufacturing method thereof - Google Patents
High-thermal-stability SPC (modified polyvinyl chloride) floor and manufacturing method thereof Download PDFInfo
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- E—FIXED CONSTRUCTIONS
- E04—BUILDING
- E04F—FINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
- E04F15/00—Flooring
- E04F15/02—Flooring or floor layers composed of a number of similar elements
- E04F15/10—Flooring or floor layers composed of a number of similar elements of other materials, e.g. fibrous or chipped materials, organic plastics, magnesite tiles, hardboard, or with a top layer of other materials
- E04F15/107—Flooring or floor layers composed of a number of similar elements of other materials, e.g. fibrous or chipped materials, organic plastics, magnesite tiles, hardboard, or with a top layer of other materials composed of several layers, e.g. sandwich panels
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D7/00—Producing flat articles, e.g. films or sheets
- B29D7/01—Films or sheets
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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
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
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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
- C08K3/24—Acids; Salts thereof
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- C08K2003/265—Calcium, strontium or barium carbonate
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Abstract
The invention discloses an SPC floor with high thermal stability and a manufacturing method thereof, wherein the SPC floor comprises a wear-resistant layer, a color film decorative layer and an SPC substrate layer which are sequentially arranged from top to bottom; the SPC substrate layer comprises the following components in parts by weight: 50-72 parts of polyvinyl chloride resin powder, 184-225 parts of modified heavy calcium carbonate, 10-18 parts of regenerated rubber, 15-20 parts of plasticizer, 1.2-3 parts of stabilizer and 1-3 parts of dispersant; the modified ground calcium carbonate is obtained by modifying ground calcium carbonate as a base material with a copolymer. According to the invention, the regenerated rubber is added into the SPC substrate layer, and the heavy calcium carbonate is modified, so that the finally obtained substrate has good fusion property and good thermal stability, is not easy to deform, and can greatly improve the durability of the SPC floor.
Description
Technical Field
The invention relates to the field of SPC (SPC) floors, in particular to an SPC floor with high thermal stability and a manufacturing method thereof.
Background
The SPC floor is a composite bottom plate mainly formed by combining polyvinyl chloride resin, high-filling calcium powder and various auxiliary agents. Is a novel material invented in response to national emission reduction, namely a hard SPC indoor floor. The SPC floor uses calcium powder as a main raw material, is subjected to plasticizing extrusion of a sheet, is subjected to four-roller calendering and hot compression on the color film decorative layer and the wear-resistant layer, does not contain heavy metal formaldehyde harmful substances, and has the advantages of environmental protection, low price, water resistance, moisture resistance, skid resistance, insect prevention, flame retardance, no cracking, no deformation, no pollution, easy cleaning and the like.
The SPC floor structure on the market at present is formed by combining a wear-resistant layer, a color film decoration layer and an SPC substrate layer, wherein the SPC substrate layer is formed by taking natural stone powder (calcium carbonate powder) and high polymer resin (polyvinyl chloride) as main raw materials through a hot fusion process in an extrusion molding mode. The natural stone powder and the PVC material can not generate chemical reaction during melting, so that the difference of the thermal shrinkage ratio of the two materials is large, and meanwhile, the PVC material has poor thermal stability and high dimensional shrinkage of the base material formed by hot extrusion, so that the floor has large dimensional change and is easy to generate the defects of splicing separation joint, deformation, warping and the like.
Disclosure of Invention
In order to solve the problems that the dimensional change of the SPC floor is large, and the defects of splicing crack, deformation, warping and the like are easily caused due to high dimensional shrinkage of a base material formed by hot extrusion of the SPC floor in the prior art, the invention aims to provide the SPC floor with high thermal stability and the manufacturing method thereof.
The purpose of the invention is realized by adopting the following technical scheme:
in a first aspect, the invention provides an SPC floor with high thermal stability, which comprises a wear-resistant layer, a color film decorative layer and an SPC substrate layer which are sequentially arranged from top to bottom; the SPC substrate layer comprises the following components in parts by weight:
50-72 parts of polyvinyl chloride resin powder, 184-225 parts of modified heavy calcium carbonate, 10-18 parts of regenerated rubber, 15-20 parts of plasticizer, 1.2-3 parts of stabilizer and 1-3 parts of dispersant;
the modified ground calcium carbonate is obtained by modifying ground calcium carbonate as a base material with a copolymer.
Preferably, the preparation method of the modified heavy calcium carbonate comprises the following steps:
m1, weighing heavy calcium carbonate, mixing with absolute ethyl alcohol, performing ultrasonic homogenization, adding bis (2-hydroxyethyl) -3-aminopropyltriethoxysilane, and stirring at 25-30 ℃ for 3-5 hours to obtain hydroxylated heavy calcium carbonate; wherein the mass ratio of the heavy calcium carbonate, the bis (2-hydroxyethyl) -3-aminopropyltriethoxysilane to the absolute ethyl alcohol is 1: 0.2-0.5: 10-15;
m2, mixing hydroxylated heavy calcium carbonate with toluene, uniformly dispersing, adding triethylamine, then placing a reaction system at 0-5 ℃, dropwise adding an acryloyl chloride solution while stirring, completely dropwise adding, heating to 25-30 ℃, keeping the temperature and stirring for 3-4 h, filtering, washing the solid with a saturated sodium carbonate solution for at least three times, washing with pure water for at least three times, and drying under reduced pressure to obtain a heavy calcium carbonate primary modified product; the mass ratio of the hydroxylated heavy calcium carbonate to the toluene to the acryloyl chloride solution is 1: 5-8: 2.4-3.6, the acryloyl chloride solution is obtained by mixing acryloyl chloride and toluene according to the mass ratio of 1: 3-5, and the addition amount of triethylamine is 5-10% of the mass of the hydroxylated heavy calcium carbonate;
m3, weighing acrylonitrile, adding the acrylonitrile into deionized water, stirring until the acrylonitrile is completely dissolved, adding a heavy calcium carbonate primary modified product, stirring and mixing uniformly, adjusting the pH value of a reaction system to 2-3, adding potassium persulfate, heating to 35-55 ℃, stirring for 2-5 hours, adjusting the pH value of the reaction system to 10-11, filtering, collecting a solid product, washing to be neutral, and drying to obtain modified heavy calcium carbonate; wherein the mass ratio of the acrylonitrile to the deionized water is 1: 8-12, the mass ratio of the heavy calcium carbonate primary modified product to the deionized water is 1: 4-6, and the addition amount of the potassium persulfate is 5-8% of the mass of the heavy calcium carbonate primary modified product.
Preferably, the regenerated rubber is prepared by sequentially carrying out microwave desulfurization and ultrasonic desulfurization on waste rubber powder.
Preferably, the microwave power of the microwave desulfurization is 550-650W, the microwave frequency is 1000-2000 MHz, and the microwave time is 3-5 min; the ultrasonic power of the ultrasonic desulfurization is 500-600W, and the ultrasonic time is 3-5 min.
Preferably, the plasticizer is one of tributyl citrate, trioctyl citrate, tributyl acetyl citrate and trioctyl acetyl citrate.
Preferably, the stabilizer is a calcium zinc stabilizer.
Preferably, the dispersant is polyethylene wax.
In a second aspect, the present invention provides a method for manufacturing an SPC floor with high thermal stability, comprising the following steps:
step 1, weighing all components of an SPC substrate layer according to the amount, placing the components in a stirrer, uniformly mixing, and then sequentially carrying out extrusion molding, cooling, cutting and polishing to obtain the SPC substrate layer;
and 2, sequentially pressing a color film decoration layer and a wear-resistant layer above the SPC substrate layer, and then finishing to obtain the SPC floor with high thermal stability.
Preferably, in the step 1, the temperature of the stirrer is set to be 130-140 ℃, and the stirring time is 0.2-0.5 h.
Preferably, in the step 1, the mixture is uniformly mixed in a stirrer, cooled to 40-50 ℃, and then placed in an extruder for extrusion molding.
The invention has the beneficial effects that:
the invention discloses an SPC floor with high thermal stability and a manufacturing method thereof, which solve the problems that a base material layer of a conventional SPC floor is easy to have poor material fusion property and poor thermal stability, and the size shrinkage rate of a base material formed by hot extrusion is high, so that the floor has large size change, and the defects of splicing gap, deformation, warping and the like are easy to generate. According to the invention, the regenerated rubber is added into the SPC substrate layer, and the heavy calcium carbonate is modified, so that the finally obtained substrate has good fusion property and good thermal stability, is not easy to deform, and can greatly improve the durability of the SPC floor.
The added regenerated rubber is obtained by activating and regenerating waste rubber powder. The waste rubber powder is granular powder prepared by mechanically crushing waste rubber, has a compact cross-linked network structure, but the surface of the waste rubber used by people for a long time loses activity, so that the waste rubber powder has poor compatibility with other materials after being recycled, and the performance of the composite material is not ideal.
In order to improve the compatibility of the heavy calcium carbonate and the polyvinyl chloride resin used in the invention, the invention obtains the modified heavy calcium carbonate by using a unique coating method. In the prior art, a surface coating polymer of calcium carbonate is used, but because the coating is formed by simply polymerizing a monomer on the surface of the calcium carbonate, the coating of the calcium carbonate coated by polymerization is not uniform, so that the effect of the calcium carbonate coated by polymerization is not expected. Finally, according to test results, the method disclosed by the invention can be better than the existing coating effect, and has better effects on the fusion degree of the polyvinyl chloride resin and the improvement of the thermal stability of the polyvinyl chloride resin.
The mechanism for preparing the modified heavy calcium carbonate is that a layer of uniformly distributed monomer is firstly manufactured on the surface of the heavy calcium carbonate, and then the monomer and the monomer capable of cooperating are copolymerized, so that a layer of uniform coating is obtained on the surface of the heavy calcium carbonate, and the compatibility of the heavy calcium carbonate and matrix resin can be further enhanced. Firstly, bis (2-hydroxyethyl) -3-aminopropyltriethoxysilane containing hydroxyl groups is used for treating heavy calcium carbonate to obtain hydroxylated heavy calcium carbonate with rich hydroxyl groups on the surface, acryloyl chloride and hydroxylated heavy calcium carbonate are mixed under an alkaline condition based on the reaction mechanism of acyl chloride groups and hydroxyl groups, and a primary modified product of the heavy calcium carbonate is obtained after the reaction; then, a mechanism of copolymerization of acrylonitrile and acrylic acid radical is used, an initiator and corresponding reaction conditions are set, and finally, the modified heavy calcium carbonate is obtained after drying treatment.
Drawings
The invention is further illustrated by means of the attached drawings, but the embodiments in the drawings do not constitute any limitation to the invention, and for a person skilled in the art, other drawings can be obtained on the basis of the following drawings without inventive effort.
FIG. 1 is an SEM image of an SPC substrate layer prepared in example 1 of the present invention;
fig. 2 is an SEM image of the SPC substrate layer prepared in comparative example 2.
Detailed Description
For the purpose of more clearly illustrating the present invention and more clearly understanding the technical features, objects and advantages of the present invention, the technical solutions of the present invention will now be described in detail below, but are not to be construed as limiting the implementable scope of the present invention.
The invention is further described with reference to the following examples.
Example 1
An SPC floor with high thermal stability comprises a wear-resistant layer, a color film decorative layer and an SPC substrate layer which are sequentially arranged from top to bottom; the SPC substrate layer comprises the following components in parts by weight:
65 parts of polyvinyl chloride resin powder, 212 parts of modified heavy calcium carbonate, 15 parts of regenerated rubber, 18 parts of tributyl citrate, 2.2 parts of a calcium-zinc stabilizer and 2 parts of polyethylene wax;
the preparation method of the modified heavy calcium carbonate comprises the following steps:
m1, weighing heavy calcium carbonate, mixing with absolute ethyl alcohol, performing ultrasonic homogenization, adding bis (2-hydroxyethyl) -3-aminopropyltriethoxysilane, and stirring at 25-30 ℃ for 3-5 hours to obtain hydroxylated heavy calcium carbonate; wherein the mass ratio of the heavy calcium carbonate, the bis (2-hydroxyethyl) -3-aminopropyltriethoxysilane to the absolute ethyl alcohol is 1:0.4: 12;
m2, mixing hydroxylated heavy calcium carbonate with toluene, uniformly dispersing, adding triethylamine, then placing a reaction system at 0-5 ℃, dropwise adding an acryloyl chloride solution while stirring, completely dropwise adding, heating to 25-30 ℃, keeping the temperature and stirring for 3-4 h, filtering, washing the solid with a saturated sodium carbonate solution for at least three times, washing with pure water for at least three times, and drying under reduced pressure to obtain a heavy calcium carbonate primary modified product; the mass ratio of the hydroxylated heavy calcium carbonate to the toluene to the acryloyl chloride solution is 1:6.5:3.2, the acryloyl chloride solution is obtained by mixing acryloyl chloride and toluene according to the mass ratio of 1:4, and the addition amount of triethylamine is 8% of the mass of the hydroxylated heavy calcium carbonate;
m3, weighing acrylonitrile, adding the acrylonitrile into deionized water, stirring until the acrylonitrile is completely dissolved, adding a heavy calcium carbonate primary modified product, stirring and mixing uniformly, adjusting the pH value of a reaction system to 2-3, adding potassium persulfate, heating to 35-55 ℃, stirring for 2-5 hours, adjusting the pH value of the reaction system to 10-11, filtering, collecting a solid product, washing to be neutral, and drying to obtain modified heavy calcium carbonate; wherein the mass ratio of the acrylonitrile to the deionized water is 1:10, the mass ratio of the heavy calcium carbonate primary modified product to the deionized water is 1:5, and the addition amount of the potassium peroxodisulfate is 6.5 percent of the mass of the heavy calcium carbonate primary modified product.
The regenerated rubber is prepared by sequentially carrying out microwave desulfurization and ultrasonic desulfurization on waste rubber powder, and specifically comprises the following steps: microwave power for microwave desulfurization is 600W, microwave frequency is 1500MHz, and microwave time is 4 min; the ultrasonic power of ultrasonic desulfurization is 550W, and the ultrasonic time is 4 min.
The manufacturing method of the SPC floor with high thermal stability comprises the following steps:
step 1, weighing all components of an SPC substrate layer according to the amount, placing the components in a stirrer, uniformly mixing, and then sequentially carrying out extrusion molding, cooling, cutting and polishing to obtain the SPC substrate layer; wherein the temperature of the stirrer is set to be 135 ℃, and the stirring time is 0.3 h;
2, sequentially pressing a color film decoration layer and a wear-resistant layer above the SPC substrate layer, and then carrying out finishing treatment to obtain the SPC floor with high thermal stability; wherein, the components are uniformly mixed in a stirrer, cooled to 40-50 ℃ and then placed in an extruder for extrusion molding.
Example 2
An SPC floor with high thermal stability comprises a wear-resistant layer, a color film decorative layer and an SPC substrate layer which are sequentially arranged from top to bottom; the SPC substrate layer comprises the following components in parts by weight:
50 parts of polyvinyl chloride resin powder, 184 parts of modified heavy calcium carbonate, 10 parts of regenerated rubber, 15 parts of trioctyl citrate, 1.2 parts of calcium-zinc stabilizer and 1 part of polyethylene wax;
the preparation method of the modified heavy calcium carbonate comprises the following steps:
m1, weighing heavy calcium carbonate, mixing with absolute ethyl alcohol, performing ultrasonic homogenization, adding bis (2-hydroxyethyl) -3-aminopropyltriethoxysilane, and stirring at 25-30 ℃ for 3-5 hours to obtain hydroxylated heavy calcium carbonate; wherein the mass ratio of the heavy calcium carbonate, the bis (2-hydroxyethyl) -3-aminopropyltriethoxysilane to the absolute ethyl alcohol is 1:0.2: 10;
m2, mixing hydroxylated heavy calcium carbonate with toluene, uniformly dispersing, adding triethylamine, then placing a reaction system at 0-5 ℃, dropwise adding an acryloyl chloride solution while stirring, completely dropwise adding, heating to 25-30 ℃, keeping the temperature and stirring for 3-4 h, filtering, washing the solid with a saturated sodium carbonate solution for at least three times, washing with pure water for at least three times, and drying under reduced pressure to obtain a heavy calcium carbonate primary modified product; the mass ratio of the hydroxylated heavy calcium carbonate to the toluene to the acryloyl chloride solution is 1:5:2.4, the acryloyl chloride solution is obtained by mixing acryloyl chloride and toluene according to the mass ratio of 1:3, and the addition amount of triethylamine is 5% of the mass of the hydroxylated heavy calcium carbonate;
m3, weighing acrylonitrile, adding the acrylonitrile into deionized water, stirring until the acrylonitrile is completely dissolved, adding a heavy calcium carbonate primary modified product, stirring and mixing uniformly, adjusting the pH value of a reaction system to 2-3, adding potassium persulfate, heating to 35-55 ℃, stirring for 2-5 hours, adjusting the pH value of the reaction system to 10-11, filtering, collecting a solid product, washing to be neutral, and drying to obtain modified heavy calcium carbonate; wherein the mass ratio of the acrylonitrile to the deionized water is 1:8, the mass ratio of the heavy calcium carbonate primary modified product to the deionized water is 1:4, and the addition amount of the potassium peroxodisulfate is 5% of the mass of the heavy calcium carbonate primary modified product.
The regenerated rubber is prepared by sequentially carrying out microwave desulfurization and ultrasonic desulfurization on waste rubber powder, and specifically comprises the following steps: the microwave power of microwave desulfurization is 550W, the microwave frequency is 1000MHz, and the microwave time is 3 min; the ultrasonic wave power of ultrasonic desulfurization is 500W, and the ultrasonic time is 3 min.
The manufacturing method of the SPC floor with high thermal stability comprises the following steps:
step 1, weighing all components of an SPC substrate layer according to the amount, placing the components in a stirrer, uniformly mixing, and then sequentially carrying out extrusion molding, cooling, cutting and polishing to obtain the SPC substrate layer; wherein the temperature of the stirrer is set to be 130 ℃, and the stirring time is 0.2 h;
2, sequentially pressing a color film decoration layer and a wear-resistant layer above the SPC substrate layer, and then carrying out finishing treatment to obtain the SPC floor with high thermal stability; wherein, the components are uniformly mixed in a stirrer, cooled to 40-50 ℃ and then placed in an extruder for extrusion molding.
Example 3
An SPC floor with high thermal stability comprises a wear-resistant layer, a color film decorative layer and an SPC substrate layer which are sequentially arranged from top to bottom; the SPC substrate layer comprises the following components in parts by weight:
72 parts of polyvinyl chloride resin powder, 225 parts of modified heavy calcium carbonate, 18 parts of regenerated rubber, 20 parts of acetyl tributyl citrate, 3 parts of calcium-zinc stabilizer and 3 parts of polyethylene wax;
the preparation method of the modified heavy calcium carbonate comprises the following steps:
m1, weighing heavy calcium carbonate, mixing with absolute ethyl alcohol, performing ultrasonic homogenization, adding bis (2-hydroxyethyl) -3-aminopropyltriethoxysilane, and stirring at 25-30 ℃ for 3-5 hours to obtain hydroxylated heavy calcium carbonate; wherein the mass ratio of the heavy calcium carbonate, the bis (2-hydroxyethyl) -3-aminopropyltriethoxysilane to the absolute ethyl alcohol is 1:0.5: 15;
m2, mixing hydroxylated heavy calcium carbonate with toluene, uniformly dispersing, adding triethylamine, then placing a reaction system at 0-5 ℃, dropwise adding an acryloyl chloride solution while stirring, completely dropwise adding, heating to 25-30 ℃, keeping the temperature and stirring for 3-4 h, filtering, washing the solid with a saturated sodium carbonate solution for at least three times, washing with pure water for at least three times, and drying under reduced pressure to obtain a heavy calcium carbonate primary modified product; the mass ratio of the hydroxylated heavy calcium carbonate to the toluene to the acryloyl chloride solution is 1:8:3.6, the acryloyl chloride solution is obtained by mixing acryloyl chloride and toluene according to the mass ratio of 1:5, and the addition amount of triethylamine is 10% of the mass of the hydroxylated heavy calcium carbonate;
m3, weighing acrylonitrile, adding the acrylonitrile into deionized water, stirring until the acrylonitrile is completely dissolved, adding a heavy calcium carbonate primary modified product, stirring and mixing uniformly, adjusting the pH value of a reaction system to 2-3, adding potassium persulfate, heating to 35-55 ℃, stirring for 2-5 hours, adjusting the pH value of the reaction system to 10-11, filtering, collecting a solid product, washing to be neutral, and drying to obtain modified heavy calcium carbonate; wherein the mass ratio of the acrylonitrile to the deionized water is 1:12, the mass ratio of the heavy calcium carbonate primary modified product to the deionized water is 1:6, and the addition amount of the potassium peroxodisulfate is 8 percent of the mass of the heavy calcium carbonate primary modified product.
The regenerated rubber is prepared by sequentially carrying out microwave desulfurization and ultrasonic desulfurization on waste rubber powder, and specifically comprises the following steps: the microwave power of the microwave desulfurization is 650W, the microwave frequency is 2000MHz, and the microwave time is 5 min; the ultrasonic wave power of ultrasonic desulfurization is 600W, and the ultrasonic time is 5 min.
The manufacturing method of the SPC floor with high thermal stability comprises the following steps:
step 1, weighing all components of an SPC substrate layer according to the amount, placing the components in a stirrer, uniformly mixing, and then sequentially carrying out extrusion molding, cooling, cutting and polishing to obtain the SPC substrate layer; wherein the temperature of the stirrer is set to be 140 ℃, and the stirring time is 0.5 h;
2, sequentially pressing a color film decoration layer and a wear-resistant layer above the SPC substrate layer, and then carrying out finishing treatment to obtain the SPC floor with high thermal stability; wherein, the components are uniformly mixed in a stirrer, cooled to 40-50 ℃ and then placed in an extruder for extrusion molding.
Comparative example 1
An SPC substrate layer comprises the following components in parts by weight:
65 parts of polyvinyl chloride resin powder, 212 parts of ground limestone, 15 parts of regenerated rubber, 18 parts of tributyl citrate, 2.2 parts of a calcium-zinc stabilizer and 2 parts of polyethylene wax;
the regenerated rubber is prepared by sequentially carrying out microwave desulfurization and ultrasonic desulfurization on waste rubber powder, and specifically comprises the following steps: microwave power for microwave desulfurization is 600W, microwave frequency is 1500MHz, and microwave time is 4 min; the ultrasonic power of ultrasonic desulfurization is 550W, and the ultrasonic time is 4 min.
The manufacturing method of the SPC floor with high thermal stability comprises the following steps:
step 1, weighing all components of an SPC substrate layer according to the amount, placing the components in a stirrer, uniformly mixing, and then sequentially carrying out extrusion molding, cooling, cutting and polishing to obtain the SPC substrate layer; wherein the temperature of the stirrer is set to be 130-140 ℃, and the stirring time is 0.2-0.5 h;
2, sequentially pressing a color film decoration layer and a wear-resistant layer above the SPC substrate layer, and then carrying out finishing treatment to obtain the SPC floor with high thermal stability; wherein, the components are uniformly mixed in a stirrer, cooled to 40-50 ℃ and then placed in an extruder for extrusion molding.
Comparative example 2
An SPC floor with high thermal stability comprises a wear-resistant layer, a color film decorative layer and an SPC substrate layer which are sequentially arranged from top to bottom; the SPC substrate layer comprises the following components in parts by weight:
65 parts of polyvinyl chloride resin powder, 212 parts of modified heavy calcium carbonate, 15 parts of regenerated rubber, 18 parts of tributyl citrate, 2.2 parts of a calcium-zinc stabilizer and 2 parts of polyethylene wax;
the preparation method of the modified heavy calcium carbonate comprises the following steps:
weighing acrylonitrile and acrylic acid, adding the acrylonitrile and the acrylic acid into deionized water, stirring until the acrylonitrile and the acrylic acid are completely dissolved, adding heavy calcium carbonate, stirring and mixing uniformly, adjusting the pH value of a reaction system to 2-3, adding potassium persulfate, heating to 35-55 ℃, stirring for 2-5 hours, adjusting the pH value of the reaction system to 10-11, filtering, collecting a solid product, washing to be neutral, and drying to obtain modified heavy calcium carbonate; wherein the mass ratio of the acrylonitrile to the acrylic acid to the deionized water is 1:1:10, the mass ratio of the ground calcium carbonate to the deionized water is 1:5, and the addition amount of the potassium peroxodisulfate is 6.5 percent of the mass of the primary modified product of the ground calcium carbonate.
The regenerated rubber is prepared by sequentially carrying out microwave desulfurization and ultrasonic desulfurization on waste rubber powder, and specifically comprises the following steps: microwave power for microwave desulfurization is 600W, microwave frequency is 1500MHz, and microwave time is 4 min; the ultrasonic power of ultrasonic desulfurization is 550W, and the ultrasonic time is 4 min.
The manufacturing method of the SPC floor with high thermal stability comprises the following steps:
step 1, weighing all components of an SPC substrate layer according to the amount, placing the components in a stirrer, uniformly mixing, and then sequentially carrying out extrusion molding, cooling, cutting and polishing to obtain the SPC substrate layer; wherein the temperature of the stirrer is set to be 135 ℃, and the stirring time is 0.3 h;
2, sequentially pressing a color film decoration layer and a wear-resistant layer above the SPC substrate layer, and then carrying out finishing treatment to obtain the SPC floor with high thermal stability; wherein, the components are uniformly mixed in a stirrer, cooled to 40-50 ℃ and then placed in an extruder for extrusion molding.
For more clearly illustrating the present invention, the SPC substrate layers prepared in examples 1 to 3 of the present invention and comparative example were compared for performance test, and the results are shown in table 1.
The detection method comprises the following steps: detecting the tensile strength by using a standard GB/T1040-92;
impact strength was measured using standard ASTM D4226;
the Vicat softening point is detected by using the standard GB/T1633-1979;
the thermal stability was tested using the standard GB/T2917.1-2002, and the thermal stability time of the SPC substrate layers of examples 1-3 and comparative examples 1-2 was tested at 200 ℃.
Table 1 performance testing of different SPC substrate layers
Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | |
Tensile Strength (MPa) | 58.8 | 57.2 | 58.4 | 51.7 | 55.2 |
Impact Strength (KJ/m)2) | 8.3 | 8.1 | 8.8 | 6.3 | 7.4 |
Vicat softening point (. degree. C.) | 92.7 | 90.6 | 93.5 | 83.9 | 88.6 |
Thermal stability time (min) | 28 | 25 | 29 | 15 | 21 |
As can be seen from table 1, the SPC substrate layers prepared in examples 1 to 3 of the present invention have better tensile strength and impact strength, which indicates that the SPC substrate layers can better resist external deformation force, have higher vicat softening point, indicate that the SPC substrate layers have stronger thermal deformation resistance, longer thermal stability time, and indicate that the continuous high temperature resistance is stronger, thereby indicating that the SPC substrate layers prepared in examples 1 to 3 of the present invention have better deformation resistance and stronger thermal stability.
In addition, SEM electron micrographs of the SPC substrate layers prepared in inventive example 1 (fig. 1) and comparative example 2 (fig. 2) are also shown, and it can be seen that the SPC substrate layer obtained in inventive example 1 has a more flat and uniform surface, and indirectly proves that the fusion degree of inventive example 1 is better.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The SPC floor with high thermal stability is characterized by comprising a wear-resistant layer, a color film decorative layer and an SPC substrate layer which are sequentially arranged from top to bottom; the SPC substrate layer comprises the following components in parts by weight:
50-72 parts of polyvinyl chloride resin powder, 184-225 parts of modified heavy calcium carbonate, 10-18 parts of regenerated rubber, 15-20 parts of plasticizer, 1.2-3 parts of stabilizer and 1-3 parts of dispersant;
the modified ground calcium carbonate is obtained by modifying ground calcium carbonate as a base material with a copolymer.
2. A high thermal stability SPC flooring according to claim 1, wherein the modified ground calcium carbonate is prepared by the method comprising:
m1, weighing heavy calcium carbonate, mixing with absolute ethyl alcohol, performing ultrasonic homogenization, adding bis (2-hydroxyethyl) -3-aminopropyltriethoxysilane, and stirring at 25-30 ℃ for 3-5 hours to obtain hydroxylated heavy calcium carbonate; wherein the mass ratio of the heavy calcium carbonate, the bis (2-hydroxyethyl) -3-aminopropyltriethoxysilane to the absolute ethyl alcohol is 1: 0.2-0.5: 10-15;
m2, mixing hydroxylated heavy calcium carbonate with toluene, uniformly dispersing, adding triethylamine, then placing a reaction system at 0-5 ℃, dropwise adding an acryloyl chloride solution while stirring, completely dropwise adding, heating to 25-30 ℃, keeping the temperature and stirring for 3-4 h, filtering, washing the solid with a saturated sodium carbonate solution for at least three times, washing with pure water for at least three times, and drying under reduced pressure to obtain a heavy calcium carbonate primary modified product; the mass ratio of the hydroxylated heavy calcium carbonate to the toluene to the acryloyl chloride solution is 1: 5-8: 2.4-3.6, the acryloyl chloride solution is obtained by mixing acryloyl chloride and toluene according to the mass ratio of 1: 3-5, and the addition amount of triethylamine is 5-10% of the mass of the hydroxylated heavy calcium carbonate;
m3, weighing acrylonitrile, adding the acrylonitrile into deionized water, stirring until the acrylonitrile is completely dissolved, adding a heavy calcium carbonate primary modified product, stirring and mixing uniformly, adjusting the pH value of a reaction system to 2-3, adding potassium persulfate, heating to 35-55 ℃, stirring for 2-5 hours, adjusting the pH value of the reaction system to 10-11, filtering, collecting a solid product, washing to be neutral, and drying to obtain modified heavy calcium carbonate; wherein the mass ratio of the acrylonitrile to the deionized water is 1: 8-12, the mass ratio of the heavy calcium carbonate primary modified product to the deionized water is 1: 4-6, and the addition amount of the potassium persulfate is 5-8% of the mass of the heavy calcium carbonate primary modified product.
3. A high thermal stability SPC floor as claimed in claim 1, wherein said reclaimed rubber is prepared from waste rubber powder by microwave desulfurization and ultrasonic desulfurization in sequence.
4. A high thermal stability SPC floor as claimed in claim 3, wherein microwave power of microwave desulfurization is 550-650W, microwave frequency is 1000-2000 MHz, and microwave time is 3-5 min; the ultrasonic power of the ultrasonic desulfurization is 500-600W, and the ultrasonic time is 3-5 min.
5. A highly thermal stable SPC floor as claimed in claim 1, wherein said plasticizer is one of tributyl citrate, trioctyl citrate, tributyl acetyl citrate, trioctyl acetyl citrate.
6. A highly thermal stable SPC floor as claimed in claim 1, wherein said stabilizer is a calcium zinc stabilizer.
7. A highly thermostable SPC floor according to claim 1, characterized in that said dispersant is polyethylene wax.
8. The method of manufacturing a SPC flooring with high thermal stability of claim 1, comprising the steps of:
step 1, weighing all components of an SPC substrate layer according to the amount, placing the components in a stirrer, uniformly mixing, and then sequentially carrying out extrusion molding, cooling, cutting and polishing to obtain the SPC substrate layer;
and 2, sequentially pressing a color film decoration layer and a wear-resistant layer above the SPC substrate layer, and then finishing to obtain the SPC floor with high thermal stability.
9. A method for manufacturing a high thermal stability SPC floor as claimed in claim 8, wherein in step 1, the temperature of the mixer is set to 130-140 ℃ and the mixing time is 0.2-0.5 h.
10. A manufacturing method of SPC floor with high thermal stability as claimed in claim 8, wherein in step 1, the mixture is mixed in a blender uniformly, cooled to 40-50 ℃ and then placed in an extruder for extrusion molding.
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CN115742506B (en) * | 2022-12-14 | 2024-09-24 | 无锡市博大竹木业有限公司 | Micro-foaming mould pressing chamfer light SPC floor and preparation process thereof |
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