CN114933856B - Flame-retardant raw lacquer and preparation method and application thereof - Google Patents
Flame-retardant raw lacquer and preparation method and application thereof Download PDFInfo
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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
- C09D193/00—Coating compositions based on natural resins; Coating compositions based on derivatives thereof
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant 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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- 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
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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
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K2003/328—Phosphates of heavy metals
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
The invention discloses a flame-retardant raw lacquer and a preparation method and application thereof, wherein the flame-retardant raw lacquer is prepared from the following raw materials in parts by weight: 80-120 parts of refined raw lacquer, 10-20 parts of acrylic resin, 5-10 parts of zirconium phosphate, 3-8 parts of modified rectorite, 3-8 parts of modified glass flake and 5-10 parts of modified titanium dioxide; the preparation method of the flame-retardant raw lacquer comprises the following steps: (1) Adding acrylic resin into refined raw lacquer according to a proportion, and then stirring for 0.5-2 min at the speed of 150rpm to obtain a solution d; (2) Adding zirconium phosphate, modified rectorite and modified titanium dioxide into the solution d according to the proportion, and stirring for 0.5-2 min at the speed of 150rpm to obtain a solution e; (3) And adding the modified glass flakes into the solution e according to the proportion, stirring at the speed of 200rpm for 0.5-2 min, and obtaining the flame-retardant raw lacquer after stirring. The invention uses raw lacquer as a direct raw material, acrylic resin as an auxiliary material, modified rectorite, glass flake and titanium dioxide are used, and zirconium phosphate is used in combination, so that the obtained material has excellent flame retardant property and good comprehensive performance.
Description
Technical Field
The invention belongs to the technical field of raw lacquer utilization, and particularly relates to flame-retardant raw lacquer and a preparation method and application thereof.
Background
Raw lacquer is one of the oldest economic tree species in China, is precious on the whole body, is a viscous liquid resin-raw lacquer which is harvested from the bark of the raw lacquer, is a natural coating and is well known as the king of the coating. The annual production of lacquer in China is about 3000 tons, which accounts for more than 80% of the total amount of the world, and the export is at the top of the world. Besides being used as the coating of general building materials, the raw lacquer can be widely used as the anticorrosive coating of industrial equipment such as national defense, machinery, petroleum, chemical engineering, mining, textile, printing and dyeing and the like, and is widely used in the restoration of furniture, coffins, artworks, musical instruments and cultural relics.
However, the direct utilization of raw lacquer may have problems of insufficient weather resistance and poor film forming property, and the reuse of raw lacquer after modification in the prior art has been widely studied, for example, tung oil, pigments, ultraviolet absorbers, nanoparticles, weather-resistant resins, etc. are added into raw lacquer, such as patent documents CN114273183A, CN108129989A, etc.; there are also methods for extracting urushiol from raw lacquer and modifying it, such as patent documents CN 110041825B and CN113265034A, but these methods have the trouble of extraction and refining, and cannot directly use the original raw lacquer.
Flame retardance is one of important properties in the using process of materials, in the prior art, reports of products with good flame retardance prepared by taking raw lacquer (non-urushiol) as a raw material are not abundant, for example, patent document CN110408319A provides a report of a flame-retardant film obtained by mixing modified ammonium polyphosphate and natural raw lacquer, but the flame retardance of the flame-retardant film is still to be further improved relatively. Due to the complex components of the raw lacquer (including urushiol, laccase, glycoprotein, moisture and other organic matters and metals) and the film forming process (the film forming mechanism is complex), how to prepare the flame-retardant raw lacquer product with good flame retardance by using the raw lacquer as a raw material is a problem worthy of systematic research.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the flame-retardant raw lacquer and the preparation method and application thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
the flame-retardant raw lacquer is prepared from the following raw materials in parts by weight:
80-120 parts of refined raw lacquer;
10-20 parts of acrylic resin;
5-10 parts of zirconium phosphate;
3-8 parts of modified rectorite;
3-8 of modified glass flakes;
5-10 parts of modified titanium dioxide.
As a further improvement of the technical scheme of the invention, the flame-retardant raw lacquer is prepared from the following raw materials in parts by weight:
100 parts of refined raw lacquer;
15 parts of acrylic resin;
8 parts of zirconium phosphate;
7 parts of modified rectorite;
6 parts of modified glass flakes;
6 parts of modified titanium dioxide.
As a further preference of the technical scheme of the invention, the preparation of the refined raw lacquer comprises the following steps: putting raw lacquer raw materials into a filter bag, and centrifuging to obtain filtrate; then, the obtained filtrate flows through a 450-mesh filter screen filled with absorbent cotton to obtain fine filtrate; and finally, stirring the fine filtrate for 8-12 h at room temperature and 60rpm, and obtaining the refined raw lacquer after stirring.
As further optimization of the technical scheme of the invention, the preparation of the modified rectorite comprises the following steps: adding sodium hydroxide into the dried rectorite raw material, uniformly mixing, calcining at 795 ℃ for 4-8 h, and grinding after calcining to obtain modified rectorite; wherein the mass ratio of the rectorite to the sodium hydroxide is 1:0.1 to 0.15.
As a further preferred embodiment of the present invention, the preparation of the modified titanium dioxide comprises the following steps: adding titanium dioxide into sodium dodecyl benzene sulfonate aqueous solution, adjusting the pH value to 5.0, stirring for 4-8 h, washing, filtering and drying after stirring to obtain modified titanium dioxide; wherein the addition amount of the titanium dioxide is 0.01-0.1 g/mL, and the concentration of the sodium dodecyl benzene sulfonate aqueous solution is 0.8wt%.
In a further preferred embodiment of the present invention, the titanium dioxide is rutile titanium dioxide.
As a further preferred embodiment of the present invention, the preparation of the modified glass flake comprises the following steps: adding the glass flake raw material into a sodium hydroxide aqueous solution, and soaking for 0.5h at 50-55 ℃; then, centrifugal separation is carried out to obtain a solid material a, and a material b is obtained after washing for multiple times by clear water; and then, adding the material b into an ethanol solution of KH550, soaking for 0.5h at room temperature, then carrying out centrifugal separation to obtain a solid material c, and drying to obtain the modified glass flake.
As a further optimization of the technical scheme of the invention, in the preparation process of the modified glass flake, the concentration of the sodium hydroxide aqueous solution is 4-8 wt%, and the concentration of KH-550 in the ethanol solution is 8-15 wt%; wherein the adding amount of the glass flakes is 0.1-0.5 g/mL.
Meanwhile, the invention also claims a preparation method of the flame-retardant raw lacquer, which comprises the following steps:
(1) Adding acrylic resin into refined raw lacquer according to a proportion, and then stirring for 0.5-2 min at the speed of 150rpm to obtain a solution d;
(2) Adding zirconium phosphate, modified rectorite and modified titanium dioxide into the solution d according to the proportion, and stirring for 0.5-2 min at the speed of 150rpm to obtain a solution e;
(3) And adding the modified glass flakes into the solution e according to the proportion, stirring at the speed of 200rpm for 0.5-2 min, and obtaining the flame-retardant raw lacquer after stirring.
Meanwhile, the invention also claims the application of the flame-retardant raw lacquer in the flame retardance of furniture, coffins or pianos.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention takes raw lacquer (non-urushiol) as a direct raw material, and adds a small amount of acrylic resin as an auxiliary material, so that the defect of poor weather resistance of the raw lacquer can be greatly improved; meanwhile, in order to endow the raw lacquer with flame retardance, the modified rectorite, the glass flakes and the titanium dioxide are used, the zirconium phosphate is used, and a plurality of substances are used in a synergistic effect, so that the prepared flame-retardant raw lacquer is excellent in flame retardance, excellent in film forming property, mechanical property and corrosion resistance and excellent in comprehensive performance.
(2) The refined raw lacquer used in the invention is subjected to primary filtration, fine filtration and stirring treatment in sequence, so that impurities in the raw lacquer can be greatly filtered, and the purity of the raw lacquer is improved; meanwhile, the stirring treatment can also increase the contact between the raw lacquer and air, accelerate the polymerization reaction in the raw lacquer and properly reduce the water content of the raw lacquer.
(3) In the modification of raw lacquer, mineral substances such as montmorillonite and kaolin are commonly used at present, which can improve the weather resistance of a coating film, but if mineral substances such as montmorillonite and kaolin are directly adopted, the width-thickness ratio is large, so that the mineral substances are difficult to be fully mixed and dispersed in acrylic resin and raw lacquer. After systematic screening and comparison, the applicant finds that the product performance obtained by adding the modified rectorite into the refined raw lacquer is better. The reason is that: the processed rectorite can destroy the layered structure, is amorphous, is fully dispersed in the refined raw lacquer, avoids agglomeration, improves the film-forming property and the mechanical property, and has good flame retardant effect.
(4) After the rutile type titanium dioxide is modified, the surface hydrophobicity of the titanium dioxide can be improved, the dispersity of the rutile type titanium dioxide in refined raw lacquer is improved, agglomeration is avoided, and the improvement of the mechanical strength, the adhesive force, the ageing resistance and other properties of the flame-retardant raw lacquer product is promoted.
(5) The invention modifies the glass flakes, can improve the wettability and the dispersibility of the glass flakes in raw lacquer and acrylic resin, the glass flakes can be distributed in a sheet shape in a system, the modified titanium dioxide and the modified rectorite can be distributed among the sheet-shaped glass flakes in a dispersion way and are distributed in an irregular filling way together, and the modified titanium dioxide and the modified rectorite are matched with each other, thereby greatly delaying the circulation of air and the permeability of corrosive media and having the functions of flame retardance and corrosion resistance.
(6) A small amount of zirconium phosphate is added, the zirconium phosphate is a good flame retardant substance, and the modified rectorite, the modified titanium dioxide and the modified glass flakes are added, so that on one hand, the connection strength of the flame-retardant raw lacquer can be improved, the coating is dense, and the heat insulation effect is achieved; on the other hand, zirconium phosphate, modified rectorite, modified titanium dioxide and modified glass flakes are used as inorganic substances, can be used as internal crosslinking sites of refined raw lacquer and acrylic resin, and can play a role in dispersion strengthening in the external combustion process. In a word, the combined action of the substances can reduce the permeability of the combustion-supporting substance, and has a synergistic flame-retardant effect, and the application prospect is wide.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
In the invention, the acrylic resin is purchased from Shanghai Kayin chemical Co., ltd; the raw lacquer raw material is the paint of the Enshi dam in Hubei province.
Example 1
The flame-retardant raw lacquer is prepared from the following raw materials in parts by weight:
100g of refined raw lacquer;
15g of acrylic resin;
8g of zirconium phosphate;
7g of modified rectorite;
6g of modified glass flakes;
6g of modified titanium dioxide.
Wherein, the preparation of the refined raw lacquer comprises the following steps: putting raw lacquer raw materials into a filter bag, and centrifuging to obtain filtrate; then, the obtained filtrate flows through a 450-mesh filter screen filled with absorbent cotton to obtain fine filtrate; and finally, stirring the fine filtrate at room temperature and 60rpm for 8 hours, and obtaining the refined raw lacquer after stirring.
The preparation method of the modified rectorite comprises the following steps: adding 1g of sodium hydroxide into 10g of dried rectorite raw material, uniformly mixing, calcining at 795 ℃ for 4h, and grinding after calcining to obtain the modified rectorite.
The preparation method of the modified titanium dioxide comprises the following steps: adding 2g of rutile titanium dioxide into 40mL of sodium dodecyl benzene sulfonate aqueous solution (0.8 wt%), adjusting the pH to 5.0, stirring for 4 hours, and washing, filtering and drying after stirring to obtain the modified titanium dioxide.
The preparation method of the modified glass flake comprises the following steps: 1.5g of glass flake raw material is added into 10mL of sodium hydroxide aqueous solution (4 wt percent) and soaked for 0.5h at 50 ℃; then, centrifugal separation is carried out to obtain a solid material a, and a material b is obtained after washing for many times by clear water; and then, adding the material b into 35mL KH550 ethanol solution (9 wt%), soaking for 0.5h at room temperature, then carrying out centrifugal separation to obtain a solid material c, and drying to obtain the modified glass flake.
In this embodiment, a preparation method of the flame-retardant raw lacquer is further provided, which includes the following steps:
(1) Adding acrylic resin into refined raw lacquer in proportion, and stirring for 1min at the speed of 150rpm to obtain a solution d;
(2) Adding zirconium phosphate, modified rectorite and modified titanium dioxide into the solution d according to the proportion, and stirring for 0.5min at the speed of 150rpm to obtain a solution e;
(3) And (3) adding the modified glass flakes into the solution e according to the proportion, stirring for 0.5min at the speed of 200rpm, and obtaining the flame-retardant raw lacquer after stirring.
Example 2
The flame-retardant raw lacquer is prepared from the following raw materials in parts by weight:
90g of refined raw lacquer;
12g of acrylic resin;
7g of zirconium phosphate;
4g of modified rectorite;
4g of modified glass flake;
5g of modified titanium dioxide.
Wherein, the preparation of the refined raw lacquer comprises the following steps: putting raw lacquer raw materials into a filter bag, and centrifuging to obtain filtrate; then, the obtained filtrate flows through a 450-mesh filter screen filled with absorbent cotton to obtain fine filtrate; and finally, stirring the fine filtrate at room temperature and 60rpm for 10 hours, and obtaining the refined raw lacquer after stirring.
The preparation method of the modified rectorite comprises the following steps: adding 1.2g of sodium hydroxide into 10g of dried rectorite raw material, uniformly mixing, calcining at 795 ℃ for 4.5h, and grinding after calcining to obtain the modified rectorite.
The preparation method of the modified titanium dioxide comprises the following steps: adding 1.2g of rutile titanium dioxide into 40mL of sodium dodecyl benzene sulfonate aqueous solution (0.8 wt%), adjusting the pH value to 5.0, stirring for 4 hours, washing, filtering and drying after stirring is finished to obtain the modified titanium dioxide.
The preparation method of the modified glass flake comprises the following steps: 1.2g of glass flake raw material is added into 10mL of sodium hydroxide aqueous solution (5 wt percent) and soaked for 0.5h at 55 ℃; then, centrifugal separation is carried out to obtain a solid material a, and a material b is obtained after washing for multiple times by clear water; and then, adding the material b into 35mL ethanol solution (10 wt%) of KH550, soaking for 0.5h at room temperature, then carrying out centrifugal separation to obtain a solid material c, and drying to obtain the modified glass flakes.
In this embodiment, a preparation method of the flame-retardant raw lacquer is further provided, which includes the following steps:
(1) Adding acrylic resin into refined raw lacquer in proportion, and stirring at the speed of 150rpm for 1.5min to obtain a solution d;
(2) Adding zirconium phosphate, modified rectorite and modified titanium dioxide into the solution d according to the proportion, and stirring for 0.5min at the speed of 150rpm to obtain a solution e;
(3) And (3) adding the modified glass flakes into the solution e according to the proportion, stirring for 0.5min at the speed of 200rpm, and obtaining the flame-retardant raw lacquer after stirring.
Example 3
The flame-retardant raw lacquer is prepared from the following raw materials in parts by weight:
110g of refined raw lacquer;
17g of acrylic resin;
9g of zirconium phosphate;
8g of modified rectorite;
5g of modified glass flakes;
7g of modified titanium dioxide.
Wherein, the preparation of the refined raw lacquer comprises the following steps: putting raw lacquer raw materials into a filter bag, and centrifuging to obtain filtrate; then, the obtained filtrate flows through a 450-mesh filter screen filled with absorbent cotton to obtain fine filtrate; and finally, stirring the fine filtrate at room temperature and 60rpm for 12 hours, and obtaining the refined raw lacquer after stirring.
The preparation method of the modified rectorite comprises the following steps: adding 1.8g of sodium hydroxide into 10g of dried rectorite raw material, uniformly mixing, calcining at 795 ℃ for 5h, and grinding after calcining to obtain the modified rectorite.
The preparation method of the modified titanium dioxide comprises the following steps: adding 2.5g of rutile titanium dioxide into 40mL of sodium dodecyl benzene sulfonate aqueous solution (0.8 wt%), adjusting the pH to 5.0, stirring for 5 hours, washing, filtering and drying after stirring to obtain the modified titanium dioxide.
The preparation method of the modified glass flake comprises the following steps: 2.2g of glass flake raw material is added into 10mL of sodium hydroxide aqueous solution (6 wt percent) and soaked for 0.5h at 55 ℃; then, centrifugal separation is carried out to obtain a solid material a, and a material b is obtained after washing for multiple times by clear water; and then, adding the material b into 35mL KH550 ethanol solution (11 wt%), soaking for 0.5h at room temperature, then carrying out centrifugal separation to obtain a solid material c, and drying to obtain the modified glass flake.
In this embodiment, a preparation method of the flame-retardant raw lacquer is further provided, which includes the following steps:
(1) Adding acrylic resin into refined raw lacquer in proportion, and stirring at the speed of 150rpm for 1.5min to obtain a solution d;
(2) Adding zirconium phosphate, modified rectorite and modified titanium dioxide into the solution d according to the proportion, and stirring for 0.5min at the speed of 150rpm to obtain a solution e;
(3) And (3) adding the modified glass flakes into the solution e according to the proportion, stirring at the speed of 200rpm for 0.5min, and obtaining the flame-retardant raw lacquer after stirring.
Comparative example 1
The flame-retardant raw lacquer is prepared from the following raw materials in parts by weight:
100g of refined raw lacquer;
15g of acrylic resin;
8g of zirconium phosphate;
7g of rectorite;
6g of modified glass flakes;
6g of modified titanium dioxide.
Wherein, the preparation of the refined raw lacquer comprises the following steps: putting raw lacquer raw materials into a filter bag, and centrifuging to obtain filtrate; then, the obtained filtrate flows through a 450-mesh filter screen filled with absorbent cotton to obtain fine filtrate; and finally, stirring the fine filtrate at room temperature and 60rpm for 8 hours, and obtaining the refined raw lacquer after stirring.
The preparation method of the modified titanium dioxide comprises the following steps: adding 2g of rutile titanium dioxide into 40mL of sodium dodecyl benzene sulfonate aqueous solution (0.8 wt%), adjusting the pH to 5.0, stirring for 4 hours, and washing, filtering and drying after stirring to obtain the modified titanium dioxide.
The preparation method of the modified glass flake comprises the following steps: 1.5g of glass flake raw material is added into 10mL of sodium hydroxide aqueous solution (4 wt percent) and soaked for 0.5h at 50 ℃; then, centrifugal separation is carried out to obtain a solid material a, and a material b is obtained after washing for many times by clear water; and then, adding the material b into 35mL ethanol solution (9 wt%) of KH550, soaking for 0.5h at room temperature, then carrying out centrifugal separation to obtain a solid material c, and drying to obtain the modified glass flakes.
In the comparative example, a preparation method of the flame-retardant raw lacquer is also provided, which comprises the following steps:
(1) Adding acrylic resin into refined raw lacquer in proportion, and stirring for 1min at the speed of 150rpm to obtain a solution d;
(2) Adding zirconium phosphate, rectorite and modified titanium dioxide into the solution d according to the proportion, and stirring for 0.5min at the speed of 150rpm to obtain a solution e;
(3) And (3) adding the modified glass flakes into the solution e according to the proportion, stirring for 0.5min at the speed of 200rpm, and obtaining the flame-retardant raw lacquer after stirring.
In comparison with example 1, rectorite in comparative example 1 was not modified.
Comparative example 2
The flame-retardant raw lacquer is prepared from the following raw materials in parts by weight:
100g of refined raw lacquer;
15g of acrylic resin;
8g of zirconium phosphate;
7g of modified rectorite;
6g of glass flakes;
6g of modified titanium dioxide.
Wherein, the preparation of the refined raw lacquer comprises the following steps: putting raw lacquer raw materials into a filter bag, and centrifuging to obtain filtrate; then, the obtained filtrate flows through a 450-mesh filter screen filled with absorbent cotton to obtain fine filtrate; and finally, stirring the fine filtrate at room temperature and 60rpm for 8 hours, and obtaining the refined raw lacquer after stirring.
The preparation method of the modified rectorite comprises the following steps: adding 1g of sodium hydroxide into 10g of dried rectorite raw material, uniformly mixing, calcining at 795 ℃ for 4h, and grinding after calcining to obtain the modified rectorite.
The preparation method of the modified titanium dioxide comprises the following steps: adding 2g of rutile titanium dioxide into 40mL of sodium dodecyl benzene sulfonate aqueous solution (0.8 wt%), adjusting the pH value to 5.0, stirring for 4 hours, washing, filtering and drying after stirring is finished to obtain the modified titanium dioxide.
In this comparative example, there is also provided a method for preparing the above flame-retardant raw lacquer, comprising the steps of:
(1) Adding acrylic resin into refined raw lacquer in proportion, and stirring for 1min at the speed of 150rpm to obtain a solution d;
(2) Adding zirconium phosphate, modified rectorite and modified titanium dioxide into the solution d according to the proportion, and stirring for 0.5min at the speed of 150rpm to obtain a solution e;
(3) And (3) adding the glass flakes into the solution e according to the proportion, stirring for 0.5min at the speed of 200rpm, and obtaining the flame-retardant raw lacquer after stirring.
In comparison with example 1, the glass flake in comparative example 2 was not modified.
Comparative example 3
The flame-retardant raw lacquer is prepared from the following raw materials in parts by weight:
100g of refined raw lacquer;
15g of acrylic resin;
8g of zirconium phosphate;
6g of modified glass flakes;
6g of modified titanium dioxide.
Wherein, the preparation of the refined raw lacquer comprises the following steps: putting raw lacquer raw materials into a filter bag, and centrifuging to obtain filtrate; then, the obtained filtrate flows through a 450-mesh filter screen filled with absorbent cotton to obtain fine filtrate; and finally, stirring the fine filtrate at room temperature and 60rpm for 8 hours, and obtaining the refined raw lacquer after stirring.
The preparation method of the modified titanium dioxide comprises the following steps: adding 2g of rutile titanium dioxide into 40mL of sodium dodecyl benzene sulfonate aqueous solution (0.8 wt%), adjusting the pH to 5.0, stirring for 4 hours, and washing, filtering and drying after stirring to obtain the modified titanium dioxide.
The preparation method of the modified glass flake comprises the following steps: 1.5g of glass flake raw material is added into 10mL of sodium hydroxide aqueous solution (4 wt percent) and soaked for 0.5h at 50 ℃; then, centrifugal separation is carried out to obtain a solid material a, and a material b is obtained after washing for multiple times by clear water; and then, adding the material b into 35mL ethanol solution (9 wt%) of KH550, soaking for 0.5h at room temperature, then carrying out centrifugal separation to obtain a solid material c, and drying to obtain the modified glass flakes.
In the comparative example, a preparation method of the flame-retardant raw lacquer is also provided, which comprises the following steps:
(1) Adding acrylic resin into refined raw lacquer in proportion, and stirring for 1min at the speed of 150rpm to obtain a solution d;
(2) Adding zirconium phosphate and modified titanium dioxide into the solution d according to the proportion, and stirring for 0.5min at the speed of 150rpm to obtain a solution e;
(3) And (3) adding the modified glass flakes into the solution e according to the proportion, stirring for 0.5min at the speed of 200rpm, and obtaining the flame-retardant raw lacquer after stirring.
In comparison with example 1, no modified rectorite was added in comparative example 3.
Comparative example 4
The flame-retardant raw lacquer is prepared from the following raw materials in parts by weight:
100g of refined raw lacquer;
15g of acrylic resin;
8g of zirconium phosphate;
7g of modified rectorite;
6g of modified titanium dioxide.
Wherein, the preparation of the refined raw lacquer comprises the following steps: putting raw lacquer raw materials into a filter bag, and centrifuging to obtain filtrate; then, the obtained filtrate flows through a 450-mesh filter screen filled with absorbent cotton to obtain fine filtrate; and finally, stirring the fine filtrate at room temperature and 60rpm for 8 hours, and obtaining the refined raw lacquer after stirring.
The preparation method of the modified rectorite comprises the following steps: adding 1g of sodium hydroxide into 10g of dried rectorite raw material, uniformly mixing, calcining at 795 ℃ for 4h, and grinding after calcining to obtain the modified rectorite.
The preparation method of the modified titanium dioxide comprises the following steps: adding 2g of rutile titanium dioxide into 40mL of sodium dodecyl benzene sulfonate aqueous solution (0.8 wt%), adjusting the pH to 5.0, stirring for 4 hours, and washing, filtering and drying after stirring to obtain the modified titanium dioxide.
In the comparative example, a preparation method of the flame-retardant raw lacquer is also provided, which comprises the following steps:
(1) Adding acrylic resin into refined raw lacquer in proportion, and stirring for 1min at the speed of 150rpm to obtain a solution d;
(2) And adding the zirconium phosphate, the modified rectorite and the modified titanium dioxide into the solution d according to the proportion, and stirring for 0.5min at the speed of 150rpm to obtain the flame-retardant raw lacquer.
In comparison with example 1, no modified glass flake was added in comparative example 4.
The flame-retardant raw lacquer products prepared in examples 1 to 2 and comparative examples 1 to 4 were subjected to a performance test. Wherein the oxygen index is determined with reference to GB/T5454-1997; flame retardancy is tested with reference to UL-94; the drying time is determined by reference to GB/T1728-2020; adhesion is determined by reference to GB/T1720-2020; the impact resistance is determined by reference to GB/T1732-2020; the alkali resistance is determined by reference to GB/T9274-1988; the high temperature resistance is determined by reference to GB/T1735-2009; the salt spray resistance is determined by reference to GB/T1771-2007; artificial aging resistance is determined by reference to GB/T1865-2009. The test results are shown in table 1.
TABLE 1 flame-retardant raw lacquer Performance test results
| Example 1 | Example 2 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | |
| Oxygen index | 38.2 | 37.6 | 27.9 | 26.2 | 24.1 | 22.8 |
| Flame retardancy | V-0 | V-0 | V-1 | V-1 | V-2 | V-2 |
| Drying time/h | 12 | 14h | 22 | 24 | 28 | 31 |
| Impact resistance/(kg/cm) | 65 | 68 | 45 | 47 | 36 | 33 |
| Adhesion/grade | 0 | 0 | 1 | 1 | 1 | 1 |
| Alkali resistance/h | 120 | 125 | 97 | 90 | 85 | 76 |
| High temperature/DEG C resistance | 480 | 490 | 430 | 420 | 400 | 390 |
| Salt spray resistance per hour | ≥1100 | ≥1100 | 980 | 950 | 810 | 760 |
| Artificial aging resistance/h | ≥500 | ≥500 | 420 | 400 | 390 | 360 |
Wherein, the specific conditions of the alkali resistance test are as follows: soaking in 30% sodium hydroxide at 100 deg.C;
wherein, the specific conditions of the high temperature resistance test are as follows: and (5) 20h.
As can be seen from Table 1, the flame-retardant raw lacquer prepared by the embodiment of the invention has excellent comprehensive performance.
The technical idea of the present invention is illustrated by the above embodiments, but the present invention is not limited to the above embodiments, that is, it does not mean that the present invention must depend on the above embodiments to be implemented. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitution of individual materials for the product of the present invention and addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (6)
1. The flame-retardant raw lacquer is characterized by being prepared from the following raw materials in parts by weight:
refining 80-120 parts of raw lacquer;
10-20 parts of acrylic resin;
5 to 10 parts of zirconium phosphate;
3 to 8 parts of modified rectorite;
3-8 parts of modified glass flakes;
5 to 10 parts of modified titanium dioxide;
the preparation method of the modified rectorite comprises the following steps: adding sodium hydroxide into the dried rectorite raw material, uniformly mixing, calcining at 795 ℃ for 4 to 8h, and grinding after calcining to obtain modified rectorite; wherein the mass ratio of the rectorite to the sodium hydroxide is 1:0.1 to 0.15;
the preparation method of the modified titanium dioxide comprises the following steps: adding titanium dioxide into a sodium dodecyl benzene sulfonate aqueous solution, adjusting the pH value to 5.0, stirring for 4 to 8 hours, washing, filtering and drying after stirring to obtain modified titanium dioxide; wherein the addition amount of the titanium dioxide is 0.01 to 0.1g/mL, and the concentration of the sodium dodecyl benzene sulfonate aqueous solution is 0.8wt%;
the preparation method of the modified glass flake comprises the following steps: adding the glass flake raw material into a sodium hydroxide aqueous solution, and soaking for 0.5h at 50-55 ℃; then, centrifugal separation is carried out to obtain a solid material a, and a material b is obtained after washing for multiple times by clear water; then, adding the material b into an ethanol solution of KH550, soaking for 0.5h at room temperature, then performing centrifugal separation to obtain a solid material c, and drying to obtain modified glass flakes;
wherein, the preparation of the refined raw lacquer comprises the following steps: putting raw lacquer raw materials into a filter bag, and centrifuging to obtain filtrate; then, the obtained filtrate flows through a 450-mesh filter screen filled with absorbent cotton to obtain fine filtrate; and finally, stirring the fine filtrate for 8 to 12h at room temperature and 60rpm, and obtaining the refined raw lacquer after stirring.
2. The flame-retardant raw lacquer as claimed in claim 1, which is prepared from the following raw materials in parts by weight:
100 parts of refined raw lacquer;
15 parts of acrylic resin;
8 parts of zirconium phosphate;
7 parts of modified rectorite;
6 parts of modified glass flakes;
6 parts of modified titanium dioxide.
3. A fire retardant raw lacquer according to claim 1, characterized in that the titanium dioxide is rutile titanium dioxide.
4. The flame-retardant raw lacquer as claimed in claim 1, wherein in the preparation process of the modified glass flakes, the concentration of the aqueous solution of sodium hydroxide is 4 to 8wt%, and the concentration of KH-550 in the ethanol solution is 8 to 15wt%; wherein the adding amount of the glass flakes is 0.1 to 0.5g/mL.
5. A method for preparing the flame-retardant raw lacquer as claimed in any one of claims 1 to 4, which is characterized by comprising the following steps:
(1) Adding acrylic resin into refined raw lacquer according to a proportion, and then stirring for 0.5-2min at a speed of 150rpm to obtain a solution d;
(2) Adding zirconium phosphate, modified rectorite and modified titanium dioxide into the solution d according to the proportion, and stirring at the speed of 150rpm for 0.5 to 2min to obtain a solution e;
(3) And adding the modified glass flakes into the solution e according to the proportion, stirring for 0.5-2min at the speed of 200rpm, and obtaining the flame-retardant raw lacquer after stirring.
6. Use of the flame retardant raw lacquer of any one of claims 1 to 4 in the flame retardant of furniture, coffins or pianos.
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