CN111393085B - Environment-friendly diatom ooze and preparation method thereof - Google Patents
Environment-friendly diatom ooze and preparation method thereof Download PDFInfo
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Abstract
The invention discloses environment-friendly diatom ooze which is characterized by comprising the following components in parts by weight: 30-50 parts of modified diatomite, 0.5-2.5 parts of black phosphorus quantum dots, 8-12 parts of palygorskite powder, 6-8 parts of illite powder, 10-20 parts of surface modified Ti-Nd-O, 0.3-0.6 part of dispersing agent, 3-6 parts of humidity regulator and 25-35 parts of water. The invention also discloses a preparation method of the environment-friendly diatom ooze. The environment-friendly diatom ooze disclosed by the invention is low in cost, long in service life, safe, fireproof, good in air purification, moisture absorption and moisture release effects, excellent in wear resistance, high in hardness, and safe and environment-friendly in use and preparation processes.
Description
Technical Field
The invention relates to the technical field of decorative materials, and particularly relates to environment-friendly diatom ooze and a preparation method thereof.
Background
In recent years, with the development of social economy and the improvement of living standard of people, the understanding of environmental problems is deepened gradually, the desire of improving the home environment is more and more urgent, and the environmental protection importance degree of decorative materials is higher and higher. However, artificial boards such as plywood and veneer boards, adhesives such as urea-formaldehyde resin, phenol-formaldehyde resin and formaldehyde resin, decorative materials such as various veneer impregnating materials, wall coatings, wallpaper, floors and chemical fiber carpets on the market can not be separated from formaldehyde, and the decorative materials contain formaldehyde and harmful gases such as formaldehyde released in the later period, so that the harm to the health of human bodies is very great. How to improve the environmental protection of the existing decoration materials becomes a difficult problem to be solved urgently in the industry.
The diatom ooze is an interior wall environment-friendly decorative wall material taking diatomite as a main raw material. The environment-friendly wall surface decorative paint has the properties of mud, is pure natural, healthy and environment-friendly, is convenient to repair and clean, is suitable for various indoor and outdoor decoration projects due to rich texture patterns and colors, is not easy to be infected with dust, and has the functions of eliminating formaldehyde, purifying air, adjusting humidity, releasing negative oxygen ions, preventing fire and retarding flame, self-cleaning the wall surface, sterilizing and deodorizing, and the like. Diatom ooze is widely popular with people. Meanwhile, various texture effects can be created through different craftsmanship treatments, and the decorative material is an ideal wall decorative material integrating environmental protection function and artistic modeling.
The diatom ooze on the market at present has higher cost and short shelf life, causes certain economic burden for people, and can not be popularized and applied, in addition, the humidifying effect is usually not obvious, the antibacterial effect is not good, and the air purifying capacity is limited, and the diatom ooze can crack after being coated on a wall for a long time, and the existing diatom ooze decorative wall material simply uses diatomite as a formaldehyde catching agent, and the adsorption of the diatomite is a dynamic balance process of desorption and adsorption, and is released while adsorbing, so that the air purifying function is required to be further improved.
The Chinese patent with application number 201811015592.9 discloses diatom ooze, which comprises the following components in parts by weight: 6-10 parts of vinyl acetate-ethylene copolymer emulsion, 5-10 parts of silica sol, 15-25 parts of diatomite, 3-8 parts of phase change energy storage microcapsules, 1-3 parts of an antibacterial agent, 3-8 parts of calcium hydroxide, 1-2 parts of a mildew preventive, 2-4 parts of cellulose, 2-5 parts of activated carbon, 3-6 parts of formaldehyde decomposition enzyme and 30-45 parts of deionized water. According to the embodiment of the invention, a great deal of research is carried out on the components and the content of the diatom ooze, and the compounded diatom ooze has the advantages of automatic temperature adjustment and control, sterilization and mildew prevention, harmful gas removal, air freshening and health benefiting. However, the diatom ooze has low wear resistance and insufficient hardness, and the moisture absorption and release effects are required to be further improved.
Disclosure of Invention
In view of the above, the invention aims to provide the environment-friendly diatom ooze and the preparation method thereof, wherein the preparation method is simple and easy to implement, low in preparation cost, high in preparation efficiency, suitable for large-scale production, and capable of realizing the unification of economic benefits, social benefits and ecological benefits; the prepared environment-friendly diatom ooze is low in cost, long in service life, safe, fireproof, good in air purification, moisture absorption and release effects, excellent in wear resistance, high in hardness, and safe and environment-friendly in use and preparation processes.
In order to achieve the purpose, the invention adopts the technical scheme that:
the environment-friendly diatom ooze is characterized by comprising the following components in parts by weight: 30-50 parts of modified diatomite, 0.5-2.5 parts of black phosphorus quantum dots, 8-12 parts of palygorskite powder, 6-8 parts of illite powder, 10-20 parts of surface modified Ti-Nd-O, 0.3-0.6 part of dispersing agent, 3-6 parts of humidity regulator and 25-35 parts of water.
Preferably, the preparation method of the black phosphorus quantum dot is as follows: example 1 of chinese invention patent CN 201811275750.4.
Preferably, the dispersant is at least one of hydroxypropyl methyl cellulose and polyvinyl alcohol.
Preferably, the humidity regulator is at least one of a sodium polyacrylate super absorbent resin, a starch grafted acrylate super absorbent resin and a cross-linked hydroxyethyl cellulose grafted acrylamide polymer super absorbent resin.
Preferably, the preparation method of the surface modified Ti-Nd-O comprises the following steps:
adding a chemically pure titanium source and a chemically pure rubidium source into ethanol, carrying out ultrasonic stirring for 0.5-1h, then slowly adding sodium acetate, carrying out intensive stirring for 1-2h, transferring the solution into a polyvinyl fluoride lined hydrothermal reaction kettle, and carrying out reaction for 15-20h at 180 ℃ and 220 ℃. Taking out the reaction kettle, repeatedly washing with deionized water and absolute ethyl alcohol after the reaction system is cooled, finally drying in a vacuum drying box at 70-80 ℃ for 18-24 hours, burning for 3-5 hours in the atmosphere of nitrogen or inert gas at 600 ℃ under 500-plus-one temperature, cooling to room temperature, grinding and crushing, and sieving with a sieve of 300-plus-one mesh and 500-mesh, wherein the obtained product is Ti-Nd-O;
and II, dispersing the Ti-Nd-O prepared in the step I in ethanol, adding N-trimethoxysilylpropyl-N, N-trimethyl ammonium chloride, stirring and reacting at 60-80 ℃ for 3-5 hours, adding 2,4, 6-tri (4-carboxyphenyl) -1,3, 5-triazine, continuously keeping the temperature and stirring for 1-2 hours, and then performing rotary evaporation to remove ethanol to obtain the surface modified Ti-Nd-O.
Preferably, the mass ratio of the titanium source, the rubidium source, the ethanol and the sodium acetate in the step I is 1:0.1 (20-30) to 2-3; the titanium source is at least one of titanium chloride, titanium nitrate and titanium sulfate; the rubidium source is at least one of rubidium chloride, rubidium nitrate and rubidium sulfate.
Preferably, in the step II, the mass ratio of the Ti-Nd-O, the ethanol, the nitrogen-trimethoxysilylpropyl-nitrogen, the nitrogen-trimethyl ammonium chloride and the 2,4, 6-tri (4-carboxyphenyl) -1,3, 5-triazine is 1 (3-5) to 0.2-0.3 to 0.1.
Preferably, the preparation method of the modified diatomite comprises the following steps:
step D1, dispersing diatomite in ethanol, adding 2-chloroethyl triethoxysilane, stirring at 60-80 ℃ for reaction for 3-5 hours, and then performing rotary evaporation to remove ethanol to obtain an intermediate product;
and D2, adding the intermediate product prepared in the step D1, the calixazole and the basic catalyst into N-methylpyrrolidone, stirring and reacting for 3-5 hours at the temperature of 80-90 ℃, centrifuging, washing for 3-6 times by using water, and drying in a vacuum drying oven at the temperature of 80-90 ℃ to constant weight to obtain the modified diatomite.
Preferably, the mass ratio of the diatomite, the ethanol and the 2-chloroethyl triethoxysilane in the step D1 is 1 (4-6) to (0.2-0.3); in the step D2, the mass ratio of the intermediate product, the calixazole, the basic catalyst and the N-methylpyrrolidone is 1 (0.1-0.2) to 0.2 (4-6).
Preferably, the preparation method of the calixazole is as follows: example 3 of chinese invention patent CN 201510309211.8; the alkaline catalyst is at least one of sodium hydride and potassium tert-butyl alkoxide.
Another objective of the present invention is to provide a method for preparing the environment-friendly diatom ooze, which is characterized by comprising the following steps: mixing the components according to the parts by weight, adding the mixture into a high-speed dispersion machine, and stirring the mixture for 15 to 30 minutes at the rotating speed of 900-1200r/min to obtain the finished product of the environment-friendly diatom ooze.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in:
(1) the preparation method of the environment-friendly diatom ooze provided by the invention is simple and feasible, low in preparation cost, high in preparation efficiency, suitable for large-scale production, and capable of realizing the unification of economic benefits, social benefits and ecological benefits.
(2) The environment-friendly diatom ooze provided by the invention overcomes the defects that the traditional diatom ooze is high in cost and short in quality guarantee period, causes a certain economic burden to people, cannot be popularized and applied, is not obvious in humidifying effect, poor in antibacterial effect and limited in air purifying capacity, can crack after being coated on a wall for a long time, takes the diatomite as a formaldehyde capture agent, and releases the diatomite while adsorbing to further improve the air purifying function.
(3) According to the environment-friendly diatom ooze provided by the invention, the surface of the diatomite is modified, and a calixazole structure is introduced, so that the adsorption capacity can be improved, the visible light catalytic activity is realized, and the function of efficiently purifying air is realized; in addition, the modification can also be beneficial to the dispersion of the composite material, so that the agglomeration is avoided.
(4) According to the environment-friendly diatom ooze provided by the invention, the black phosphorus quantum dots are added and have a synergistic effect with other components, so that the air purification effect can be effectively improved; the addition of the palygorskite powder and the illite powder can improve the hardness of the diatom ooze and also can play a role in bonding; the surface modification Ti-Nd-O improves the response range of visible light and the effect of removing formaldehyde by photocatalysis through heterogeneous doping, and can also improve the wettability, the moisture absorption and the moisture removal performance through surface modification, thereby effectively preventing the cracking phenomenon in the long-term use process.
Detailed Description
In order to make the technical solutions of the present invention better understood and make the above features, objects, and advantages of the present invention more comprehensible, the present invention is further described with reference to the following examples. The examples are intended to illustrate the invention only and are not intended to limit the scope of the invention.
In the embodiment of the invention, the raw materials are all purchased commercially; the preparation method of the black phosphorus quantum dot is as follows: example 1 of chinese invention patent CN 201811275750.4; the preparation method of the calixazole is described in the following: example 3 of chinese invention patent CN 201510309211.8.
Example 1
The environment-friendly diatom ooze is characterized by comprising the following components in parts by weight: 30 parts of modified diatomite, 0.5 part of black phosphorus quantum dots, 8 parts of palygorskite powder, 6 parts of illite powder, 10 parts of surface-modified Ti-Nd-O, 0.3 part of hydroxypropyl methyl cellulose, 3 parts of sodium polyacrylate super absorbent resin and 25 parts of water.
The preparation method of the surface modified Ti-Nd-O comprises the following steps:
i, adding chemically pure titanium chloride and rubidium nitrate into ethanol, carrying out ultrasonic stirring for 0.5h, then slowly adding sodium acetate, carrying out vigorous stirring for 1h, transferring the solution into a hydrothermal reaction kettle with a polyvinyl fluoride lining, and carrying out reaction for 15h at 180 ℃. Taking out the reaction kettle, repeatedly washing the reaction system with deionized water and absolute ethyl alcohol after the reaction system is cooled, finally drying the reaction system in a vacuum drying oven at 70 ℃ for 18 hours, burning the reaction system for 3 hours in a nitrogen atmosphere at 500 ℃, cooling the reaction system to room temperature, grinding and crushing the reaction system, and sieving the reaction system by using a 300-mesh sieve to obtain a product, namely Ti-Nd-O; the mass ratio of the titanium chloride to the rubidium nitrate to the ethanol to the sodium acetate is 1:0.1:20: 2;
II, dispersing the Ti-Nd-O prepared in the step I in ethanol, adding N-trimethoxysilylpropyl-N, N-trimethyl ammonium chloride, stirring and reacting at 60 ℃ for 3 hours, then adding 2,4, 6-tri (4-carboxyphenyl) -1,3, 5-triazine, continuing to keep the temperature and stirring for 1 hour, and then performing rotary evaporation to remove ethanol to obtain surface modified Ti-Nd-O; the mass ratio of the Ti-Nd-O, the ethanol, the N-trimethoxysilylpropyl-N, the N-trimethyl ammonium chloride and the 2,4, 6-tri (4-carboxyphenyl) -1,3, 5-triazine is 1:3:0.2: 0.1.
The preparation method of the modified diatomite comprises the following steps:
step D1, dispersing diatomite in ethanol, adding 2-chloroethyl triethoxysilane, stirring at 60 ℃ for reaction for 3 hours, and then performing rotary evaporation to remove ethanol to obtain an intermediate product; the mass ratio of the diatomite to the ethanol to the 2-chloroethyl triethoxysilane is 1:4: 0.2;
d2, adding the intermediate product prepared in the step D1, dicarbazole and sodium hydride into N-methylpyrrolidone, stirring and reacting for 3 hours at 80 ℃, centrifuging, washing for 3 times by using water, and drying in a vacuum drying oven at 80 ℃ to constant weight to obtain modified diatomite; the mass ratio of the intermediate product to the calixazole to the sodium hydride to the N-methylpyrrolidone is 1:0.1:0.2: 4.
The preparation method of the environment-friendly diatom ooze is characterized by comprising the following steps: mixing the components in parts by weight, adding the mixture into a high-speed dispersion machine, and stirring the mixture for 15min at the rotating speed of 900r/min to obtain the finished product of the environment-friendly diatom ooze.
Example 2
The environment-friendly diatom ooze is characterized by comprising the following components in parts by weight: 35 parts of modified diatomite, 1 part of black phosphorus quantum dots, 9 parts of palygorskite powder, 6.5 parts of illite powder, 12 parts of surface-modified Ti-Nd-O, 0.4 part of polyvinyl alcohol, 4 parts of starch grafted acrylate super absorbent resin and 27 parts of water.
The preparation method of the surface modified Ti-Nd-O comprises the following steps:
i, adding chemically pure titanium nitrate and rubidium sulfate into ethanol, carrying out ultrasonic stirring for 0.7h, then slowly adding sodium acetate, carrying out intensive stirring for 1.2h, transferring the solution into a hydrothermal reaction kettle with a polyvinyl fluoride lining, and carrying out reaction for 17h at 190 ℃. Taking out the reaction kettle, repeatedly washing the reaction system with deionized water and absolute ethyl alcohol after the reaction system is cooled, finally drying the reaction system in a vacuum drying oven at 73 ℃ for 20 hours, burning the reaction system for 3.5 hours in a helium atmosphere at 530 ℃, cooling the reaction system to room temperature, grinding and crushing the reaction system, and sieving the reaction system by a 350-mesh sieve to obtain a product, namely Ti-Nd-O; the mass ratio of the titanium nitrate to the rubidium sulfate to the ethanol to the sodium acetate is 1:0.1:22: 2.3;
II, dispersing the Ti-Nd-O prepared in the step I in ethanol, adding N-trimethoxysilylpropyl-N, N-trimethyl ammonium chloride, stirring and reacting at 65 ℃ for 3.5 hours, then adding 2,4, 6-tri (4-carboxyphenyl) -1,3, 5-triazine, continuing to keep the temperature and stirring for 1.2 hours, and then performing rotary evaporation to remove ethanol to obtain surface modified Ti-Nd-O; the mass ratio of the Ti-Nd-O, the ethanol, the N-trimethoxysilylpropyl-N, the N-trimethyl ammonium chloride and the 2,4, 6-tri (4-carboxyphenyl) -1,3, 5-triazine is 1:3.5:0.22: 0.1.
The preparation method of the modified diatomite comprises the following steps:
step D1, dispersing diatomite in ethanol, adding 2-chloroethyl triethoxysilane, stirring at 65 ℃ for reaction for 3.5 hours, and then performing rotary evaporation to remove ethanol to obtain an intermediate product; the mass ratio of the diatomite to the ethanol to the 2-chloroethyl triethoxysilane is 1:4.5: 0.23;
d2, adding the intermediate product prepared in the step D1, the calixazole and the potassium tert-butyl alkoxide into N-methylpyrrolidone, stirring and reacting for 3.5 hours at 83 ℃, centrifuging, washing for 4 times by using water, and drying in a vacuum drying oven at 82 ℃ to constant weight to obtain modified diatomite; the mass ratio of the intermediate product to the calixazole to the potassium tert-butyl alkoxide to the N-methylpyrrolidone is 1:0.12:0.2: 4.5;
the preparation method of the environment-friendly diatom ooze is characterized by comprising the following steps: mixing the components in parts by weight, adding the mixture into a high-speed dispersion machine, and stirring the mixture for 20min at the rotating speed of 1000r/min to obtain the finished product of the environment-friendly diatom ooze.
Example 3
The environment-friendly diatom ooze is characterized by comprising the following components in parts by weight: 40 parts of modified diatomite, 1.5 parts of black phosphorus quantum dots, 10 parts of palygorskite powder, 7 parts of illite powder, 15 parts of surface-modified Ti-Nd-O, 0.45 part of hydroxypropyl methyl cellulose, 4.5 parts of cross-linked hydroxyethyl cellulose grafted acrylamide polymer super absorbent resin and 30 parts of water.
The preparation method of the surface modified Ti-Nd-O comprises the following steps:
i, adding chemically pure titanium sulfate and rubidium chloride into ethanol, carrying out ultrasonic stirring for 0.7h, then slowly adding sodium acetate, carrying out intensive stirring for 1.5h, transferring the solution into a hydrothermal reaction kettle with a polyvinyl fluoride lining, and carrying out reaction for 18h at 200 ℃. Taking out the reaction kettle, repeatedly washing the reaction system with deionized water and absolute ethyl alcohol after the reaction system is cooled, finally drying the reaction system in a vacuum drying oven at the temperature of 75 ℃ for 21 hours, burning the reaction system for 4 hours in a neon atmosphere at the temperature of 55 ℃, cooling the reaction system to the room temperature, grinding and crushing the reaction system, and sieving the reaction system by a sieve of 400 meshes to obtain a product, namely Ti-Nd-O; the mass ratio of the titanium sulfate to the rubidium chloride to the ethanol to the sodium acetate is 1:0.1:25: 2.5;
II, dispersing the Ti-Nd-O prepared in the step I in ethanol, adding N-trimethoxysilylpropyl-N, N-trimethyl ammonium chloride, stirring and reacting for 4 hours at 70 ℃, then adding 2,4, 6-tri (4-carboxyphenyl) -1,3, 5-triazine, continuing to keep the temperature and stirring for 1.5 hours, and then performing rotary evaporation to remove ethanol to obtain surface modified Ti-Nd-O; the mass ratio of the Ti-Nd-O, the ethanol, the N-trimethoxysilylpropyl-N, the N-trimethyl ammonium chloride and the 2,4, 6-tri (4-carboxyphenyl) -1,3, 5-triazine is 1:4:0.25: 0.1.
The preparation method of the modified diatomite comprises the following steps:
step D1, dispersing diatomite in ethanol, adding 2-chloroethyl triethoxysilane, stirring at 70 ℃ for reaction for 4 hours, and then performing rotary evaporation to remove ethanol to obtain an intermediate product; the mass ratio of the diatomite to the ethanol to the 2-chloroethyl triethoxysilane is 1:5: 0.25;
d2, adding the intermediate product prepared in the step D1, dicarbazole and sodium hydride into N-methylpyrrolidone, stirring and reacting for 4 hours at 85 ℃, centrifuging, washing for 3-6 times by using water, and drying in a vacuum drying oven at 85 ℃ to constant weight to obtain modified diatomite; the mass ratio of the intermediate product to the calixazole to the sodium hydride to the N-methylpyrrolidone is 1:0.15:0.2: 5;
the preparation method of the environment-friendly diatom ooze is characterized by comprising the following steps: mixing the components in parts by weight, adding the mixture into a high-speed dispersion machine, and stirring the mixture for 22min at the rotating speed of 1050r/min to obtain the finished product of the environment-friendly diatom ooze.
Example 4
The environment-friendly diatom ooze is characterized by comprising the following components in parts by weight: 45 parts of modified diatomite, 2 parts of black phosphorus quantum dots, 11 parts of palygorskite powder, 7.5 parts of illite powder, 18 parts of surface-modified Ti-Nd-O, 0.5 part of dispersing agent, 5 parts of humidity regulator and 32 parts of water.
The dispersing agent is formed by mixing hydroxypropyl methyl cellulose and polyvinyl alcohol according to a mass ratio of 3: 5; the humidity regulator is formed by mixing sodium polyacrylate super absorbent resin, starch grafted acrylate super absorbent resin and cross-linked hydroxyethyl cellulose grafted acrylamide polymer super absorbent resin according to the mass ratio of 1:2: 3.
The preparation method of the surface modified Ti-Nd-O comprises the following steps:
i, adding a chemically pure titanium source and a chemically pure rubidium source into ethanol, carrying out ultrasonic stirring for 0.9h, then slowly adding sodium acetate, carrying out intensive stirring for 1.8h, transferring the solution into a hydrothermal reaction kettle with a polyvinyl fluoride lining, and carrying out reaction for 19h at 210 ℃. Taking out the reaction kettle, repeatedly washing the reaction system with deionized water and absolute ethyl alcohol after the reaction system is cooled, finally drying the reaction system in a vacuum drying oven at 78 ℃ for 23 hours, burning the reaction system for 4.7 hours in an argon atmosphere at 580 ℃, cooling the reaction system to room temperature, grinding and crushing the reaction system, and sieving the reaction system with a sieve of 450 meshes to obtain a product Ti-Nd-O; the mass ratio of the titanium source to the rubidium source to the ethanol to the sodium acetate is 1:0.1:28: 2.8; the titanium source is formed by mixing titanium chloride, titanium nitrate and titanium sulfate according to the mass ratio of 1:3: 2; the rubidium source is formed by mixing rubidium chloride, rubidium nitrate and rubidium sulfate according to the mass ratio of 2:3: 1;
II, dispersing the Ti-Nd-O prepared in the step I in ethanol, adding N-trimethoxysilylpropyl-N, N-trimethyl ammonium chloride, stirring and reacting for 4.5 hours at 77 ℃, then adding 2,4, 6-tri (4-carboxyphenyl) -1,3, 5-triazine, continuing to keep the temperature and stirring for 1.8 hours, and then performing rotary evaporation to remove ethanol to obtain surface modified Ti-Nd-O; the mass ratio of the Ti-Nd-O, the ethanol, the N-trimethoxysilylpropyl-N, the N-trimethyl ammonium chloride and the 2,4, 6-tri (4-carboxyphenyl) -1,3, 5-triazine is 1:4.5:0.28: 0.1.
The preparation method of the modified diatomite comprises the following steps:
step D1, dispersing diatomite in ethanol, adding 2-chloroethyl triethoxysilane, stirring at 78 ℃ for reaction for 4.5 hours, and then performing rotary evaporation to remove ethanol to obtain an intermediate product; the mass ratio of the diatomite to the ethanol to the 2-chloroethyl triethoxysilane is 1:5.7: 0.28;
d2, adding the intermediate product prepared in the step D1, the calixazole and the basic catalyst into N-methylpyrrolidone, stirring and reacting for 4.5 hours at 88 ℃, centrifuging, washing for 5 times by using water, and drying in a vacuum drying oven at 88 ℃ to constant weight to obtain modified diatomite; the mass ratio of the intermediate product to the calixazole to the basic catalyst to the N-methylpyrrolidone is 1:0.18:0.2: 5.8; the alkaline catalyst is formed by mixing sodium hydride and tert-butyl potassium alcoholate according to the mass ratio of 3: 5.
The preparation method of the environment-friendly diatom ooze is characterized by comprising the following steps: mixing the components in parts by weight, adding the mixture into a high-speed dispersion machine, and stirring the mixture for 28min at the rotating speed of 1100r/min to obtain the finished product of the environment-friendly diatom ooze.
Example 5
The environment-friendly diatom ooze is characterized by comprising the following components in parts by weight: 50 parts of modified diatomite, 2.5 parts of black phosphorus quantum dots, 12 parts of palygorskite powder, 8 parts of illite powder, 20 parts of surface-modified Ti-Nd-O, 0.6 part of polyvinyl alcohol, 6 parts of sodium polyacrylate super absorbent resin and 35 parts of water.
The preparation method of the surface modified Ti-Nd-O comprises the following steps:
i, adding chemically pure titanium nitrate and rubidium chloride into ethanol, carrying out ultrasonic stirring for 1 hour, then slowly adding sodium acetate, carrying out intensive stirring for 2 hours, transferring the solution into a polyvinyl fluoride lined hydrothermal reaction kettle, and carrying out reaction for 20 hours at 220 ℃. Taking out the reaction kettle, repeatedly washing the reaction system with deionized water and absolute ethyl alcohol after the reaction system is cooled, finally drying the reaction system in a vacuum drying oven at the temperature of 80 ℃ for 24 hours, then firing the reaction system for 5 hours in the atmosphere of nitrogen at the temperature of 600 ℃, cooling the reaction system to room temperature, grinding and crushing the reaction system, and sieving the reaction system by a sieve of 500 meshes to obtain a product, namely Ti-Nd-O; the mass ratio of the titanium nitrate to the rubidium chloride to the ethanol to the sodium acetate is 1:0.1:30: 3;
II, dispersing the Ti-Nd-O prepared in the step I in ethanol, adding N-trimethoxysilylpropyl-N, N-trimethyl ammonium chloride, stirring and reacting for 5 hours at 80 ℃, then adding 2,4, 6-tri (4-carboxyphenyl) -1,3, 5-triazine, continuing to keep the temperature and stirring for 2 hours, and then performing rotary evaporation to remove ethanol to obtain surface modified Ti-Nd-O; the mass ratio of the Ti-Nd-O, the ethanol, the N-trimethoxysilylpropyl-N, the N-trimethyl ammonium chloride and the 2,4, 6-tri (4-carboxyphenyl) -1,3, 5-triazine is 1:5:0.3: 0.1.
The preparation method of the modified diatomite comprises the following steps:
step D1, dispersing diatomite in ethanol, adding 2-chloroethyl triethoxysilane, stirring at 80 ℃ for 5 hours, and then performing rotary evaporation to remove ethanol to obtain an intermediate product; the mass ratio of the diatomite to the ethanol to the 2-chloroethyl triethoxysilane is 1:6: 0.3;
d2, adding the intermediate product prepared in the step D1, the calixazole and the potassium tert-butyl alkoxide into N-methylpyrrolidone, stirring and reacting for 5 hours at 90 ℃, centrifuging, washing for 6 times by using water, and drying in a vacuum drying oven at 90 ℃ to constant weight to obtain modified diatomite; the mass ratio of the intermediate product to the calixazole to the potassium tert-butyl alkoxide to the N-methylpyrrolidone is 1:0.2:0.2: 6.
The preparation method of the environment-friendly diatom ooze is characterized by comprising the following steps: mixing the components in parts by weight, adding the mixture into a high-speed dispersion machine, and stirring the mixture for 30min at the rotating speed of 1200r/min to obtain the finished product of the environment-friendly diatom ooze.
Comparative example 1
The present example provides an environment-friendly diatom ooze, which has a formulation and a preparation method substantially the same as those of example 1, except that modified diatomaceous earth is replaced with diatomaceous earth.
Comparative example 2
The present example provides an environment-friendly diatom ooze, the formulation and preparation method of which are substantially the same as those of example 1, except that Ti-Nd-O is used instead of surface-modified Ti-Nd-O.
Comparative example 3
The present example provides an environmentally friendly diatom ooze, which has a formulation and a preparation method substantially the same as those of example 1, except that no black phosphorus quantum dots are added.
Comparative example 4
The present example provides an environment-friendly diatom ooze, the formulation and preparation method of which are substantially the same as those of example 1, except that no palygorskite powder and illite powder are added.
The formaldehyde purification performance and formaldehyde purification effect durability of the examples and the comparative examples are tested according to JC/T2177-2013 Diatom ooze decorative wall material, and the test results are shown in Table 1.
TABLE 1
| Item | Formaldehyde purifying performance | Durability of formaldehyde purification effect |
| Unit of | ％ | ％ |
| Example 1 | 97 | 90 |
| Example 2 | 98 | 92 |
| Example 3 | 98 | 92 |
| Example 4 | 99 | 94 |
| Example 5 | 99 | 95 |
| Comparative example 1 | 90 | 80 |
| Comparative example 2 | 89 | 78 |
| Comparative example 3 | 92 | 81 |
| Comparative example 4 | 95 | 88 |
As can be seen from table 1, the environment-friendly diatom ooze of the embodiment of the invention has better formaldehyde purification performance and longer formaldehyde purification effect than the comparative environment-friendly diatom ooze, which is the result of the synergistic effect of the components.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (4)
1. The environment-friendly diatom ooze is characterized by comprising the following components in parts by weight: 30-50 parts of modified diatomite, 0.5-2.5 parts of black phosphorus quantum dots, 8-12 parts of palygorskite powder, 6-8 parts of illite powder, 10-20 parts of surface modified Ti-Nd-O, 0.3-0.6 part of dispersing agent, 3-6 parts of humidity regulator and 25-35 parts of water;
the preparation method of the surface modified Ti-Nd-O comprises the following steps:
i, adding a chemically pure titanium source and a chemically pure rubidium source into ethanol, carrying out ultrasonic stirring for 0.5-1h, then slowly adding sodium acetate, carrying out violent stirring for 1-2h, transferring the solution into a hydrothermal reaction kettle with a polyvinyl fluoride lining, reacting for 15-20h at the temperature of 180 ℃ plus 220 ℃, taking out the reaction kettle, repeatedly washing with deionized water and absolute ethyl alcohol after a reaction system is cooled, finally drying for 18-24 h in a vacuum drying box at the temperature of 70-80 ℃, firing for 3-5h in the atmosphere of nitrogen or inert gas at the temperature of 600 ℃ plus 500 plus, cooling to room temperature, grinding and crushing, and sieving with a sieve of 300 plus 500 meshes to obtain a product, namely Ti-Nd-O; the mass ratio of the titanium source to the rubidium source to the ethanol to the sodium acetate is 1:0.1 (20-30) to 2-3; the titanium source is at least one of titanium chloride, titanium nitrate and titanium sulfate; the rubidium source is at least one of rubidium chloride, rubidium nitrate and rubidium sulfate;
II, dispersing the Ti-Nd-O prepared in the step I in ethanol, adding N-trimethoxysilylpropyl-N, N-trimethyl ammonium chloride, stirring and reacting at 60-80 ℃ for 3-5 hours, adding 2,4, 6-tri (4-carboxyphenyl) -1,3, 5-triazine, continuously keeping the temperature and stirring for 1-2 hours, and then performing rotary evaporation to remove ethanol to obtain surface modified Ti-Nd-O; the mass ratio of the Ti-Nd-O, the ethanol, the N-trimethoxysilylpropyl-N, the N-trimethyl ammonium chloride and the 2,4, 6-tri (4-carboxyphenyl) -1,3, 5-triazine is 1 (3-5) to 0.2-0.3 to 0.1;
the preparation method of the modified diatomite comprises the following steps:
step D1, dispersing diatomite in ethanol, adding 2-chloroethyl triethoxysilane, stirring at 60-80 ℃ for reaction for 3-5 hours, and then performing rotary evaporation to remove ethanol to obtain an intermediate product; the mass ratio of the diatomite, the ethanol and the 2-chloroethyl triethoxysilane is 1 (4-6) to 0.2-0.3;
d2, adding the intermediate product prepared in the step D1, the calixazole and the basic catalyst into N-methylpyrrolidone, stirring and reacting for 3-5 hours at 80-90 ℃, centrifuging, washing for 3-6 times by using water, and drying in a vacuum drying oven at 80-90 ℃ to constant weight to obtain modified diatomite; the mass ratio of the intermediate product, the calixazole, the basic catalyst and the N-methylpyrrolidone is 1 (0.1-0.2) to 0.2 (4-6).
2. The environment-friendly diatom ooze according to claim 1, wherein said dispersant is at least one of hydroxypropyl methylcellulose and polyvinyl alcohol.
3. The environment-friendly diatom ooze of claim 1, wherein said moisture control agent is at least one of a sodium polyacrylate super absorbent resin, a starch grafted acrylate super absorbent resin, a cross-linked hydroxyethyl cellulose grafted acrylamide polymer super absorbent resin.
4. The environment-friendly diatom ooze of any one of claims 1-3, wherein said method of making the environment-friendly diatom ooze comprises the steps of: mixing the components according to the parts by weight, adding the mixture into a high-speed dispersion machine, and stirring the mixture for 15 to 30 minutes at the rotating speed of 900-1200r/min to obtain the finished product of the environment-friendly diatom ooze.
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