CN114369404A - Epoxy floor coating and preparation method thereof - Google Patents
Epoxy floor coating and preparation method thereof Download PDFInfo
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- CN114369404A CN114369404A CN202210025912.9A CN202210025912A CN114369404A CN 114369404 A CN114369404 A CN 114369404A CN 202210025912 A CN202210025912 A CN 202210025912A CN 114369404 A CN114369404 A CN 114369404A
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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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- 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
- C09D7/47—Levelling agents
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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
- C09D7/63—Additives non-macromolecular organic
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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
- C09D7/65—Additives macromolecular
Abstract
The application relates to the field of coatings, in particular to an epoxy floor coating and a preparation method thereof. The epoxy floor coating comprises the following components in parts by weight: 80-120 parts of silicon powder modified epoxy resin; 40-80 parts of polyamide resin; 20-40 parts of organic silicon resin; 10-25 parts of pigment and filler; 0.5-2 parts of a leveling agent; the preparation method of the silicon powder modified epoxy resin comprises the following steps: a. silicon powder pretreatment; b. and (3) modifying the epoxy resin. This application is through silica flour modified epoxy for when having surface hardness concurrently, showing the pliability that has improved the coating system, then it is difficult for taking place the fracture after the solidification film-forming, very big degree has prolonged the life of epoxy terrace coating.
Description
Technical Field
The application relates to the field of coatings, in particular to an epoxy floor coating and a preparation method thereof.
Background
The coating is a material which is coated on the surface of an object and can form a tough protective film, and the coating mainly has the functions of protection, decoration or other special functions (insulation, rust prevention, water prevention, impermeability and the like), and can be divided into the following components according to different film forming materials: natural resin-based coatings, phenol-based coatings, alkyd-based coatings, amino-based coatings, epoxy-based coatings, and the like, and among them, the most widely used epoxy-based coatings are exemplified.
The epoxy-based coating in the related art includes: the epoxy floor coating is prepared by taking epoxy resin as a main film forming substance and continuously stirring a stable dispersion formed by mixing materials. The hardness and the wear resistance of the obtained epoxy floor coating can meet the basic protection requirements of people on the epoxy floor coating.
Although the coating prepared by the above-mentioned related techniques can be directly used, the coating film has poor flexibility due to high hardness after drying, and then the surface of the coating film is easily cracked when the shrinkage force inside the coating film exceeds the cohesion of the coating film or is damaged by extrusion. Therefore, it is highly desirable to provide an epoxy floor coating that has both hardness and flexibility.
Disclosure of Invention
In order to enable the epoxy floor coating to have hardness and flexibility, the application provides the epoxy floor coating and the preparation method thereof.
First aspect, this application provides an epoxy terrace coating, adopts following technical scheme:
80-120 parts of silicon powder modified epoxy resin;
40-80 parts of polyamide resin;
20-40 parts of organic silicon resin;
10-25 parts of pigment and filler;
0.5-2 parts of a leveling agent;
the preparation method of the silicon powder modified epoxy resin comprises the following steps:
a. silicon powder pretreatment: preheating silicon powder, freeze-drying the silicon powder, putting the silicon powder into a hydrogen peroxide solution, and heating to obtain pretreated silicon powder;
b. modification of epoxy resin: and heating and mixing the pretreated silicon powder, the coupling agent and the epoxy resin to obtain the silicon powder modified epoxy resin.
By adopting the technical scheme, after the epoxy resin modified by the silicon powder is doped into an epoxy floor coating system, the flexibility of the coating after curing can be obviously enhanced, and the cross-linking state of a film forming substance can be improved, so that the epoxy floor coating can have excellent flexibility and hardness after being cured into a film;
the reason for this analysis may be: after the silicon powder is pretreated, a partial hydroxylation structure can be formed, so that the bonding performance of the surface of the silicon powder is further improved, the subsequent modification and bonding of the silicon powder with a coupling agent and epoxy resin are facilitated, the silicon powder and a film-forming structure formed by multi-component crosslinking can be fully combined and filled, a more complex and compact three-dimensional crosslinking network structure is formed, and the flexibility of the three-dimensional crosslinking network structure is greatly improved.
The solvent-free epoxy floor coating has excellent bonding strength under the action of the leveling agent, is tightly attached to a substrate to be protected, has low shrinkage rate during curing film forming, is not easy to generate pores and cracks, and reduces the cracking phenomenon caused by the fact that the internal shrinkage force after curing film forming exceeds the cohesive force of a coating film.
Preferably, the preparation steps of the silicon powder modified epoxy resin are as follows:
a. silicon powder pretreatment: preheating silicon powder to 80-100 ℃, reducing the temperature to 0 ℃ at a rate of 10-20 ℃/s, then carrying out vacuum drying on the silicon powder for 10-15min, then placing the silicon powder into 20-40% by mass of aqueous hydrogen peroxide, and heating the silicon powder for 1-2h at a temperature of 80-120 ℃ to obtain pretreated silicon powder;
b. modification of epoxy resin: mixing the pretreated silicon powder, the coupling agent and the epoxy resin, heating to 90-130 ℃, and mixing at 500-800r/min for 30-45min to obtain the silicon powder modified epoxy resin.
By adopting the technical scheme, the hydroxylated silicon dioxide with strong cohesiveness is formed on the surface of the silicon powder pretreated by the preheating, freeze drying and hydrogen peroxide immersion processes, so that the integral bonding capability of the silicon powder is remarkably improved, and the subsequent modification bonding of the silicon powder with the coupling agent and the epoxy resin is facilitated.
Preferably, the usage amount of the pretreated silicon powder, the coupling agent and the epoxy resin is 1 (0.5-0.8) to 6-10 in percentage by weight.
By adopting the technical scheme, the pre-treated silicon powder, the coupling agent and the epoxy resin in the proportion have better combined and compounded effect, and the pre-treated silicon powder can be fully dispersed and combined in a film-forming structure formed by multi-component crosslinking under the action of the coupling agent, so that a three-dimensional crosslinking network with a more complex and compact structure is formed, and the flexibility of the epoxy floor coating is obviously improved.
Preferably, the silicon powder is nano-scale micro-silicon powder, the average particle size of the nano-scale micro-silicon powder is 30nm, and the volume density of the nano-scale micro-silicon powder is 0.19g/cm3The specific surface area was 42.4m2/g。
By adopting the technical scheme, after the nano-scale silica fume with the particle size, the density and the specific surface area is pretreated, the surface bonding performance is greatly improved, and then the nano-scale silica fume can be fully combined and filled with a film forming structure in a three-dimensional cross-linked network under the action of a coupling agent.
Preferably, the coupling agent is one or more of KH-550, KH-782, TM-27 and Z-6040.
By adopting the technical scheme, the coupling agent of the components can effectively act on the silicon powder, so that the silicon powder can be fully combined and filled in a film-forming structure in a three-dimensional cross-linked network.
Preferably, the coupling agent consists of KH-550 and TM-27 in a weight ratio of 1 (3-5).
By adopting the technical scheme, the coupling agent compounded by the two components has a better coupling effect, and pretreated silicon powder can be fully combined and filled in a film-forming structure in a three-dimensional cross-linked network, so that the overall flexibility and strength of the film-forming structure are improved.
Preferably, the epoxy resin is dimer acid modified epoxy resin, the epoxy value is 200-400g/eq, and the viscosity at 25 ℃ is 400-900 mPas.
By adopting the technical scheme, the dimer acid modified epoxy resin with the epoxy value and the viscosity has better flexibility and adhesive force after being cured, and can be fully combined with silicon powder under the action of the coupling agent, so that the three-dimensional cross-linked network has excellent mechanical property.
Preferably, the pigment and filler are micron-sized fillers and are one or more of white carbon black, titanium dioxide, quartz powder and talcum powder.
By adopting the technical scheme, the pigment and filler of the components can be compounded with silicon powder besides being used as the hardness of a filler reinforced coating system, so that a better flexibility improvement effect is achieved.
Preferably, the leveling agent is one or more of KMT-5510S, KMT-5257N, KMT-5595 and KMT-7012.
By adopting the technical scheme, the flatting agent with the components can promote the coating to form a flat, smooth and uniform coating film in the drying film-forming process, and can also effectively reduce the shrinkage rate of the coating film during curing film-forming, thereby reducing the cracking phenomenon caused by the fact that the internal shrinkage force of the coating film exceeds the cohesion force of the coating film.
In a second aspect, the application provides a preparation method of an epoxy floor coating, which adopts the following technical scheme:
a preparation method of the epoxy floor coating comprises the following steps:
s1, mixing the silicon powder modified epoxy resin and the polyamide resin at the temperature of 160-220 ℃ and the temperature of 1000-2000r/min for 15-30 min;
s2, adding organic silicon resin, pigment and filler and flatting agent, mixing at 80-120 ℃ and 3000r/min for 5-15min to obtain the epoxy floor coating.
By adopting the technical scheme, the preparation steps are simple, various conditions are easy to control, and the obtained epoxy floor coating is stable and uniform in performance and has excellent strength and flexibility, so that the epoxy floor coating is suitable for large-scale industrial production.
In summary, the present application has the following beneficial effects:
1. according to the epoxy floor coating, the epoxy resin modified by the silicon powder is doped, so that the flexibility of the coating after curing is obviously enhanced, the crosslinking state of a film forming substance is improved, and the formed three-dimensional crosslinking network structure is more complex and compact, so that the epoxy floor coating after curing and film forming is endowed with excellent flexibility and hardness;
2. the epoxy resin used in the application is dimer acid modified epoxy resin, and after being cured, the epoxy resin not only has better flexibility and adhesive force, but also can be fully combined with silicon powder under the action of a coupling agent, so that the mechanical property of a film-forming structure is guaranteed;
3. the preparation method is simple and convenient, all conditions are easy to control and achieve, and the prepared epoxy floor coating is stable and uniform in performance, has excellent hardness and flexibility, and is suitable for industrial mass production.
Detailed Description
The present application will be described in further detail with reference to examples.
The raw materials used in the examples and comparative examples of the present application are commercially available except for the specific description below.
The nano-scale silicon powder, model CW-Si-001, the submicron-scale silicon powder, model CW-Si-002, are purchased from Shanghai Chaowei nanometer science and technology Limited;
epoxy resin, CAS No.: 61788-97-4;
dimer acid modified epoxy resin with CAS number 67989-52-0;
polyamide resin, CAS No.: 63428-84-2;
silicone resin, dimethyldichlorosilane, CAS No.: 75-78-5;
the pigment and the filler are micron-sized fillers, and the average particle size of the fillers is 5-10 um;
leveling agent: KMT-5510S, KMT-5257N, KMT-5595 and KMT-7012 were purchased from Kukanin New materials, Inc., of Foshan.
Preparation example
Preparation example 1
The preparation method of the silicon powder modified epoxy resin comprises the following steps:
a. silicon powder pretreatment: preheating 20kg of silicon powder to 80 ℃, reducing the temperature to 0 ℃ at a rate of 10 ℃/s, then carrying out vacuum drying on the silicon powder for 15min, then placing the silicon powder into 20 mass percent aqueous hydrogen peroxide, and heating the silicon powder for 2h at 80 ℃ to obtain pretreated silicon powder;
b. modification of epoxy resin: mixing and heating the pretreated silicon powder, the coupling agent and the epoxy resin according to the weight ratio of 1:0.3:5 to 90 ℃, and mixing at 500r/min for 30min to obtain silicon powder modified epoxy resin;
wherein the silicon powder is submicron silicon powder with average particle diameter of 120nm and volume density of 1.89g/cm3The specific surface area was 8.30m2Per gram, the coupling agent used was KH-550.
Preparation example 2
The silicon powder modified epoxy resin is the same as the preparation example 1 except for the following preparation steps:
a. silicon powder pretreatment: preheating 20kg of silicon powder to 60 ℃, reducing the temperature to 0 ℃ at a rate of 10 ℃/s, then carrying out vacuum drying on the silicon powder for 15min, then placing the silicon powder into 10 mass percent aqueous hydrogen peroxide, and heating the silicon powder for 2h at 60 ℃ to obtain pretreated silicon powder;
b. modification of epoxy resin: and mixing and heating the pretreated silicon powder, the coupling agent and the epoxy resin to 60 ℃, and mixing at 500r/min for 30min to obtain the silicon powder modified epoxy resin.
Preparation example 3
The silicon powder modified epoxy resin is the same as the preparation example 1 except for the following preparation steps:
a. silicon powder pretreatment: preheating 20kg of silicon powder to 100 ℃, reducing the temperature to 0 ℃ at a rate of 20 ℃/s, then carrying out vacuum drying on the silicon powder for 15min, then placing the silicon powder into 40 mass percent aqueous hydrogen peroxide, and heating the silicon powder for 2h at a temperature of 120 ℃ to obtain pretreated silicon powder;
b. modification of epoxy resin: and mixing and heating the pretreated silicon powder, the coupling agent and the epoxy resin to 90 ℃, and mixing at 500r/min for 30min to obtain the silicon powder modified epoxy resin.
Preparation example 4
The silicon powder modified epoxy resin is the same as the preparation example 1 except for the following preparation steps:
a. silicon powder pretreatment: preheating 20kg of silicon powder to 80 ℃, reducing the temperature to 0 ℃ at a rate of 10 ℃/s, then carrying out vacuum drying on the silicon powder for 15min, then placing the silicon powder into 20 mass percent aqueous hydrogen peroxide, and heating the silicon powder for 1h at a temperature of 90 ℃ to obtain pretreated silicon powder;
b. modification of epoxy resin: and mixing the pretreated silicon powder, the coupling agent and the epoxy resin, heating to 110 ℃, and mixing at 650r/min for 35min to obtain the silicon powder modified epoxy resin.
Preparation example 5
The silicon powder modified epoxy resin is the same as the preparation example 1 except for the following preparation steps:
a. silicon powder pretreatment: preheating 20kg of silicon powder to 120 ℃, reducing the temperature to 0 ℃ at a rate of 10 ℃/s, then carrying out vacuum drying on the silicon powder for 15min, then placing the silicon powder into a 50% aqueous hydrogen peroxide solution by mass percent, and heating the silicon powder for 2h at a temperature of 80 ℃ to obtain pretreated silicon powder;
b. modification of epoxy resin: and mixing the pretreated silicon powder, the coupling agent and the epoxy resin, heating to 150 ℃, and mixing at 1000r/min for 60min to obtain the silicon powder modified epoxy resin.
Preparation example 6
The silicon powder modified epoxy resin is the same as the preparation example 1 except that the amount of the silicon powder, the coupling agent and the epoxy resin which are pretreated in the step b is 1:0.5:6 in percentage by weight.
Preparation example 7
The silicon powder modified epoxy resin is the same as the preparation example 1 except that the amount of the silicon powder, the coupling agent and the epoxy resin which are pretreated in the step b is 1:0.6:8 in percentage by weight.
Preparation example 8
The silicon powder modified epoxy resin is the same as the preparation example 1 except that the amount of the silicon powder, the coupling agent and the epoxy resin which are pretreated in the step b is 1:0.8:10 in percentage by weight.
Preparation example 9
The silicon powder modified epoxy resin is the same as the preparation example 1 except that the amount of the silicon powder, the coupling agent and the epoxy resin which are pretreated in the step b is 1:1:20 in percentage by weight.
Preparation example 10
A silicon powder modified epoxy resin, except a, the silicon powder is nano-scale micro-silicon powder, the average particle diameter is 30 mu m, and the volume density is 0.19g/cm3The specific surface area was 42.4m2The contents other than/g were the same as in preparation example 1.
Preparation example 11
The silicon powder modified epoxy resin is the same as the preparation example 1 except that the coupling agent in the step b is TM-27.
Preparation example 12
A silicon powder modified epoxy resin is the same as that of preparation example 1 except that in b, a coupling agent consists of KH-550 and TM-27 in a weight ratio of 1:1.
Preparation example 13
A silicon powder modified epoxy resin is the same as that of preparation example 1 except that in b, a coupling agent consists of KH-550 and TM-27 in a weight ratio of 1: 3.
Preparation example 14
A silicon powder modified epoxy resin is the same as that of preparation example 1 except that in b, a coupling agent consists of KH-550 and TM-27 in a weight ratio of 1: 4.
Preparation example 15
A silicon powder modified epoxy resin is the same as that of preparation example 1 except that in b, a coupling agent consists of KH-550 and TM-27 in a weight ratio of 1: 5.
Preparation example 16
A silicon powder modified epoxy resin is the same as that of preparation example 1 except that in b, a coupling agent consists of KH-550 and TM-27 in a weight ratio of 1: 7.
Performance test
Coating films formed by curing the epoxy floor coating in the embodiment and the comparative example are selected as detection objects, the adhesive force, the hardness and the flexibility of the coating films are respectively tested, and the specific detection steps and the detection standards are as follows:
1) adhesion detection
The test is carried out according to the pull-apart method specified in GB/T5210-2006, a test column with the diameter of 20mm is adopted, the upper test column and the lower test column are coaxially butted with a test plate for testing, three groups of coating films are arranged in parallel in each group, and the average value of the test results is recorded.
2) Pencil hardness detection
The coating film is placed on a placing table of a testing machine, the testing can be carried out, the specific testing steps and the testing standards are tested according to GB/T6739-1996, the weight is 500g, and the testing results are recorded in the following table and used for evaluating the surface hardness of the material.
3) Flexibility testing
Bending the epoxy floor coating according to the detection method in GB/T1731-1993, wherein the diameters of cylinders are respectively 75, 70, 65, 60, 55, 50, 45, 40, 35 and 30 (unit is mm), bending the coating by using the cylinders, and recording the minimum diameter without cracks, wherein the smaller the diameter of the cylinder is, the stronger the flexibility of the coating is.
Examples
Example 1
The epoxy floor coating comprises the following components in parts by weight shown in Table 1, and is prepared by the following preparation method:
s1, mixing the silicon powder modified epoxy resin and the polyamide resin at 200 ℃ at 1500r/min for 25 min;
s2, adding organic silicon resin, pigment and filler and a flatting agent, and mixing at 100 ℃ and 2500r/min for 10min to obtain the epoxy floor coating;
the silicon powder modified epoxy resin is prepared by the preparation example 1, the organic silicon resin is dimethyl dichlorosilane, the pigment filler is white carbon black, and the leveling agent is KMT-5510S.
Examples 2 to 6
An epoxy floor coating, which differs from example 1 in that the components and their respective weights are shown in table 1.
TABLE 1 Components and weights (kg) thereof in examples 1-6
Comparative example 1
An epoxy floor coating was the same as in example 1 except that the epoxy resin was not modified.
Comparative example 2
An epoxy floor coating, which is different from example 1 in that the coating is the same as example 1 except that no pretreatment is performed on silicon powder.
Five groups of coating films prepared in the above examples 1 to 6 and comparative examples 1 to 2 were extracted, and adhesion, hardness and flexibility were measured according to the above measurement procedures and measurement standards, and the average values were recorded in the following table.
As can be seen from the above table, the adhesion of the epoxy floor coatings prepared in examples 1-6 is all qualified, i.e., 8.5-8.8MPa, which is higher than the standard value of 8.0 MPa; the pencil hardness is as high as 2H; the minimum diameter of the epoxy floor coating without cracks is 40-45mm, so that the epoxy floor coating prepared from the components in the proportioning range has excellent hardness and flexibility, and is not easy to crack after being cured into a film.
As can also be seen from the above table, comparative example 1 has a small decrease in hardness, only H, compared to example 1, due to the unmodified epoxy resin; the flexibility is greatly reduced, and the minimum diameter without cracks is as high as 65 mm;
the doping of the silicon powder modified epoxy resin is beneficial to enhancing the flexibility of the cured coating and improving the cross-linking state of the film forming substance, so that the epoxy terrace coating can have excellent flexibility and hardness after being cured into a film.
As can also be seen from the above table, comparative example 2 has a small decrease in flexibility and a minimum diameter of up to 55mm without cracks, compared to example 1, because the silicon powder is not pretreated;
the silicon powder is pretreated to be beneficial to the modification and combination of the silicon powder, the coupling agent and the epoxy resin, and the presumed reason is that the silicon powder surface can form a partial hydroxylation structure to further improve the combination performance of the silicon powder surface, and then the silicon powder can be fully combined and filled with a film-forming structure formed by multi-component crosslinking to form a more complex and compact three-dimensional crosslinking network structure, so that the flexibility of the three-dimensional crosslinking network structure is greatly improved.
In conclusion, the silicon powder modified epoxy resin can obviously enhance the flexibility of the cured coating and improve the crosslinking state of the film forming substance by doping, so that the epoxy floor coating can have excellent flexibility and hardness after being cured into a film;
the solvent-free epoxy floor coating has excellent bonding strength and low shrinkage rate during integral curing film forming, and is not easy to generate pores and cracks during curing film forming.
Examples 7 to 10
An epoxy floor coating is different from that in example 1 in that the silicon powder modified epoxy resin is used in different conditions, and the specific correspondence relationship is shown in the table below.
Table: comparative table of use of silicone powder-modified epoxy resins in examples 7 to 10
| Group of | Silicon powder modified epoxy resin |
| Example 7 | Prepared from preparation example 2 |
| Example 8 | Prepared from preparation example 3 |
| Example 9 | Prepared from preparation example 4 |
| Example 10 | Prepared from preparation example 5 |
Five groups of the coating films prepared in examples 7 to 10 were extracted, and the adhesion, hardness and flexibility were measured according to the above measurement procedures and measurement standards, and the average values were recorded in the following table.
As can be seen from the above table, the adhesion of the epoxy floor coatings prepared in examples 7-10 is all qualified, i.e., 8.2-8.5MPa, which is higher than the standard value of 8.0 MPa; the pencil hardness is H or 2H; the minimum diameter of the epoxy floor coating without cracks is 45-50mm, so that the epoxy floor coating prepared by the process has excellent hardness and flexibility, and is not easy to crack after being cured into a film.
Further, the epoxy floor coatings prepared in examples 1 and 8-9 have excellent hardness and flexibility, the pencil hardness is as high as 2H, and the minimum diameter without cracks is 45mm, so that the processes in preparation examples 1 and 3-4 are preferred.
In conclusion, the hydroxylated silicon dioxide with strong cohesiveness is formed on the surface of the silicon powder pretreated by the preheating, freeze drying and hydrogen peroxide immersion process conditions, so that the overall binding capacity of the silicon powder is remarkably improved, the subsequent modification binding of the silicon powder with the coupling agent and the epoxy resin is facilitated, and the mechanical property of the epoxy floor coating is further ensured.
Examples 11 to 14
An epoxy floor coating is different from that in example 1 in that the silicon powder modified epoxy resin is used in different conditions, and the specific correspondence relationship is shown in the table below.
Table: comparative table of use of silicone powder-modified epoxy resins in examples 11 to 14
| Group of | Silicon powder modified epoxy resin |
| Example 11 | Prepared from preparation example 6 |
| Example 12 | Prepared from preparation example 7 |
| Example 13 | Prepared from preparation example 8 |
| Example 14 | Prepared from preparation example 9 |
Five groups of the coating films prepared in examples 11 to 14 were extracted, and the adhesion, hardness and flexibility were measured according to the above measurement procedures and measurement standards, and the average values were recorded in the following table.
As can be seen from the above table, the adhesion of the epoxy floor coatings prepared in examples 11-14 is all qualified, i.e., 8.5-8.8MPa, which is higher than the standard value of 8.0 MPa; the pencil hardness is H or 2H; the minimum diameter of the coating without cracks is 35-45mm, so that the epoxy floor coating prepared from the silicon powder, the coupling agent and the epoxy resin which are pre-treated according to the proportion has the advantages of hardness and flexibility.
In particular, the epoxy floor coatings prepared in examples 11 to 13 have the adhesion force of 8.8MPa, excellent hardness and flexibility, the pencil hardness of 3H, and the minimum diameter of no crack of 35mm, and the performance improvement effect is most remarkable when the amounts of the pretreated silicon powder, the coupling agent and the epoxy resin in b are 1 (0.5 to 0.8) and 6 to 10 in percentage by weight.
In conclusion, the pretreated silicon powder, the coupling agent and the epoxy resin in the proportion have a good combined compounding effect, the pretreated silicon powder can be fully combined into a film-forming structure formed by multi-component crosslinking under the action of the coupling agent, and the flexibility of the epoxy floor coating is obviously improved.
Example 15
An epoxy floor coating was prepared as in example 1, except that the silica powder-modified epoxy resin used was prepared as in example 10.
Five groups of the coating films prepared in example 10 were extracted, and the adhesion, hardness and flexibility were measured according to the above measurement procedures and measurement standards, and the average values were recorded in the following table.
As can be seen from the above table, the adhesion of the epoxy floor coating prepared in example 10 is qualified, i.e., 8.6MPa, which is higher than the standard value of 8.0 MPa; the pencil hardness is as high as 3H; the minimum diameter without cracks is only 30 mm;
therefore, after the nano-scale silica fume with the particle size, the density and the specific surface area is pretreated, the surface bonding performance is greatly improved, and the nano-scale silica fume can be fully combined and filled with a film forming structure in a three-dimensional cross-linked network under the action of a coupling agent, so that the epoxy terrace film has excellent mechanical properties.
Examples 16 to 21
An epoxy floor coating is different from that in example 1 in that the silicon powder modified epoxy resin is used in different conditions, and the specific correspondence relationship is shown in the table below.
Table: comparative table of use of silicone powder-modified epoxy resins in examples 16 to 21
| Group of | Silicon powder modified epoxy resin |
| Example 16 | Prepared from preparation example 11 |
| Example 17 | Prepared from preparation example 12 |
| Example 18 | Prepared from preparation example 13 |
| Example 19 | Prepared from preparation 14 |
| Example 20 | Prepared from preparation example 15 |
| Example 21 | Prepared from preparation example 16 |
Five groups of the coating films prepared in examples 16 to 21 were extracted, and the adhesion, hardness and flexibility were measured according to the above measurement procedures and measurement standards, and the average values were recorded in the following table.
As can be seen from the above table, the adhesion of the epoxy floor coatings prepared in examples 16-21 is all qualified, i.e., 8.5-8.8MPa, which is higher than the standard value of 8.0 MPa; the pencil hardness is 2H or 3H; the minimum diameter of the epoxy floor coating without cracks is 35-45mm, so that the hardness and flexibility of the epoxy floor coating can be effectively improved by the components and the coupling agent in proportion.
Particularly, the epoxy floor coatings prepared in the examples 18 to 20 have the adhesion force of 8.8MPa, excellent hardness and flexibility, pencil hardness of 3H, and the minimum diameter of no crack of 35mm, and the coupling agent in the b is composed of KH-550 and TM-27 according to the weight ratio of 1 (3-5), so that the performance improvement effect is most remarkable.
In conclusion, the multi-component coupling agents have a synergistic compounding effect, so that the pretreated silicon powder can be more fully combined and filled in a film forming structure in a three-dimensional cross-linked network, and the coating film is endowed with excellent flexibility and strength.
Example 22
An epoxy floor coating, which is different from the embodiment 1 in that the epoxy resin is dimer acid modified epoxy resin, the epoxy value is 400g/eq, the viscosity at 25 ℃ is 400 mPas, and the rest is the same as the embodiment 1.
Five groups of the coating films prepared in example 22 were extracted, and the adhesion, hardness and flexibility were measured according to the above measurement procedures and measurement standards, and the average values were recorded in the following table.
As can be seen from the above table, the adhesion of the epoxy floor coating prepared in example 22 is qualified, i.e., 8.8MPa, which is higher than the standard value of 8.0 MPa; the pencil hardness is as high as 3H; the minimum diameter without cracks is only 30 mm;
therefore, the dimer acid modified epoxy resin with the epoxy value and the viscosity can endow the coating film with excellent hardness and adhesive force, and can be fully combined with silicon powder under the action of a coupling agent, so that the excellent mechanical property, namely the flexibility of a three-dimensional crosslinking network is guaranteed.
Example 23
An epoxy floor coating is different from the embodiment 1 in that the color filler is composed of white carbon black and titanium dioxide according to the weight ratio of 1:0.5, and the rest is the same as the embodiment 1.
Example 24
An epoxy floor coating is different from the embodiment 1 in that the color filler is composed of white carbon black, titanium dioxide and quartz powder according to the weight ratio of 1:0.3:0.2, and the rest is the same as the embodiment 1.
Five groups of the coating films prepared in examples 23 to 24 were extracted, and the adhesion, hardness and flexibility were measured according to the above measurement procedures and measurement standards, and the average values were recorded in the following table.
As can be seen from the above table, the adhesion of the epoxy floor coatings prepared in examples 23-24 is acceptable, i.e., higher than the standard value of 8.0MPa, and 8.3MPa, which is lower than that of example 1; the hardness of the pencil is as high as 3H, and compared with the case of only using white carbon black in example 1, the hardness of the pencil is further improved; the minimum diameter without cracks is only 40 mm;
therefore, the pigment and filler of the components can achieve a better improvement effect by compounding different components and cooperating with silicon powder, and the pigment and filler is an excellent filler component and can obviously enhance the hardness of a coating film.
Example 25
An epoxy floor coating is different from the epoxy floor coating in example 1 in that the leveling agent is prepared from KMT-5510S and KMT-5257N in a weight ratio of 1:2, and the rest is the same as the epoxy floor coating in example 1.
Example 26
An epoxy floor coating is different from the epoxy floor coating in example 1 in that the leveling agent is prepared from KMT-5510S, KMT-5257N and KMT-5595 in a weight ratio of 1:1.5:0.5, and the rest is the same as example 1.
Five groups of coating films prepared in the above examples 25 to 26 were extracted, and the adhesion, hardness and flexibility were measured according to the above measurement procedures and measurement standards, and the average values were recorded in the following table.
As can be seen from the above table, the adhesion of the epoxy floor coatings prepared in examples 25-26 is acceptable, i.e., 8.5-8.7MPa, which is higher than the standard value of 8.0 MPa; the pencil hardness is 2H; the minimum diameter of no crack is only 40mm, and compared with the method of only using a single leveling agent in example 1, the flexibility of the coating film is further improved;
the leveling agent with the components can promote the coating to form a flat, smooth and uniform coating film in the drying film-forming process through the compounding of multiple components, and can also effectively reduce the shrinkage rate during film forming by curing, thereby reducing the cracking phenomenon caused by film curing.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (10)
1. The epoxy floor coating is characterized by comprising the following components in parts by weight:
80-120 parts of silicon powder modified epoxy resin;
40-80 parts of polyamide resin;
20-40 parts of organic silicon resin;
10-25 parts of pigment and filler;
0.5-2 parts of a leveling agent;
the preparation method of the silicon powder modified epoxy resin comprises the following steps:
a. silicon powder pretreatment: preheating silicon powder, freeze-drying the silicon powder, putting the silicon powder into a hydrogen peroxide solution, and heating to obtain pretreated silicon powder;
b. modification of epoxy resin: and heating and mixing the pretreated silicon powder, the coupling agent and the epoxy resin to obtain the silicon powder modified epoxy resin.
2. The epoxy floor coating of claim 1, wherein the silica powder-modified epoxy resin is prepared by the following steps:
a. silicon powder pretreatment: preheating silicon powder to 80-100 ℃, reducing the temperature to 0 ℃ at a rate of 10-20 ℃/s, then carrying out vacuum drying on the silicon powder for 10-15min, then placing the silicon powder into 20-40% by mass of aqueous hydrogen peroxide, and heating the silicon powder for 1-2h at a temperature of 80-120 ℃ to obtain pretreated silicon powder;
b. modification of epoxy resin: mixing and heating the pretreated silicon powder, the coupling agent and the epoxy resin to 90-130 ℃, and mixing at the speed of 500-800r/min for 30-45min to obtain the silicon powder modified epoxy resin.
3. The epoxy floor coating of claim 1, wherein the amount of the pretreated silica powder, the coupling agent and the epoxy resin is 1 (0.5-0.8) to 6-10% by weight.
4. The epoxy floor coating of claim 1, wherein the silicon powder is nano-scale microsilica with an average particle size of 30nm and a bulk density of 0.19g/cm3The specific surface area was 42.4m2/g。
5. The epoxy floor coating of claim 1, wherein the coupling agent is one or more of KH-550, KH-782, TM-27, Z-6040.
6. The epoxy floor coating of claim 5, wherein the coupling agent consists of KH-550 and TM-27 in a weight ratio of 1 (3-5).
7. The epoxy floor coating as claimed in claim 1, wherein the epoxy resin is dimer acid modified epoxy resin with an epoxy value of 200-400g/eq and a viscosity of 400-900mPas at 25 ℃.
8. The epoxy floor coating of claim 1, wherein the color filler is a micron filler selected from one or more of white carbon black, titanium dioxide, quartz powder, and talc.
9. The epoxy floor coating of claim 1, wherein the leveling agent is one or more of KMT-5510S, KMT-5257N, KMT-5595 and KMT-7012.
10. The method of preparing the epoxy floor coating of any of claims 1-9, characterized by comprising the steps of:
s1, mixing the silicon powder modified epoxy resin and the polyamide resin at the temperature of 160-220 ℃ and the temperature of 1000-2000r/min for 15-30 min;
s2, adding organic silicon resin, pigment and filler and flatting agent, mixing at 80-120 ℃ and 3000r/min for 5-15min to obtain the epoxy floor coating.
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| JP2004269807A (en) * | 2003-03-12 | 2004-09-30 | Auto Kagaku Kogyo Kk | Thixotropic ordinary temperature-curable composition and process for producing the same |
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