CN111961364A - Preparation method of country experience type light-storing luminescent material - Google Patents
Preparation method of country experience type light-storing luminescent material Download PDFInfo
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- CN111961364A CN111961364A CN202010808534.2A CN202010808534A CN111961364A CN 111961364 A CN111961364 A CN 111961364A CN 202010808534 A CN202010808534 A CN 202010808534A CN 111961364 A CN111961364 A CN 111961364A
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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
- C09D5/22—Luminous paints
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4804—Two or more polyethers of different physical or chemical nature
- C08G18/4812—Mixtures of polyetherdiols with polyetherpolyols having at least three hydroxy groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
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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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/08—Polyurethanes from polyethers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3009—Sulfides
- C08K2003/3018—Sulfides of magnesium, calcium, strontium or barium
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Abstract
The invention provides a preparation method of a country experience type light-storing luminescent material, which comprises the following specific steps: dehydrating the mixed solution of dihydric alcohol and trihydric alcohol for 3-5h at the temperature of 100-110 ℃ and under the vacuum condition of 0.05-0.2 MPa; adding an aliphatic ketone solution and an organotin solution into the dehydrated alcohol solution, mixing, heating to 70-80 ℃, adding triphenylmethane triisocyanate, and reacting at the temperature of 70-80 ℃ for 1.5-2.5 h; and (3) adding the light-storing luminescent material in the catalytic reaction, and continuing the heat preservation reaction to obtain the single-component light-storing polyurethane luminescent material. The luminescent material prepared by the method increases the light storage luminescent function of the coating, improves the problem of the traditional fluorescent coating, increases the luminescent stability intensity, is not easy to migrate, can keep the luminescent group lasting and stable, has excellent glossiness and weather resistance, is not easy to quench, and shows the typical light storage luminescent enhancement effect.
Description
Technical Field
The invention relates to the field of luminescent coatings, in particular to a preparation method of a country experience type light-storing luminescent material.
Background
In recent years, the country vigorously implements the village revivification strategy, the village travels more and more, and the village economy has a large development space at night. A large amount of light is often used in the night economy of the tourism industry to create experience scenes, the country environment is uniformly urbanized due to the large amount of light, the country characteristics are lost, the country environment is polluted due to the use of a large amount of light, and the national ecological environment construction concept is not met.
The light-storing and self-luminous material is a novel environment-friendly material which can automatically absorb light energy in daytime and release light energy at night. If the environment-friendly luminescent material is applied to the construction of the night landscape in the village, the environment-friendly luminescent material can be used for the construction of landscape lanes, and experience type landscape wall surfaces can be laid, namely tourists can use portable mobile phones and flashlights to paint on the landscape wall surfaces coated with the light-storing self-luminescent material, so that interactive experience is generated. The method not only accords with the national ecological environment protection concept, but also can create a special landscape different from the urban night scene.
Polyurethane has been widely used in the fields of coating, adhesive, synthetic leather and the like due to its excellent properties, but along with the increase of the demand for novel functional materials in the production and life, the polyurethane is endowed with functionality, and the polyurethane has gained more and more extensive attention. The application chemical industry (12 months in 2000, No. 29, No. 4, pages 21-24) reports the preparation of a colored polyurethane waterproof coating, and colored polyurethane is obtained by a method of blending with color paste, but the product obtained by the method is a mixture, and the color paste and the polyurethane have compatibility problems, and are easy to migrate or seep in the use process, so that the color is not uniform and the depth is different, and the colored polyurethane cannot absorb light, store energy and emit light, cannot be displayed at night, and cannot achieve the feeling of interactive experience.
The long-afterglow luminescent material is used as an energy storage luminescent material, has the advantage of long luminescence time, has the function of indicating at night and can be applied to occasions such as tunnels, signs, indicating marks and the like, and can effectively solve the problems of short persistence, poor gloss and poor weather resistance of fluorescent type light display. However, the luminescent material of the long afterglow luminescent paint is usually directly blended with the organic paint, the uniformity is poor, fine particles and floccule precipitates are easy to appear, and the storage stability of the paint is also influenced to a certain extent. In addition, the coating of the type is also easy to cause uneven luminescence of the coating in the using process due to uneven blending of the luminescent material in the coating in the spraying process, so that the experience feeling is poor.
Therefore, the invention aims to design a preparation method for effectively solving the problems of nonuniform combination and easy migration of the long-afterglow luminescent material and the polyurethane coating, producing the light-storing luminescent coating with uniform color development, excellent glossiness and weather resistance, and applying the luminescent material prepared by the method to rural experience type landscapes.
Disclosure of Invention
The invention aims to provide a preparation method of a country-experience type light-storing luminescent material, which can effectively solve the problems of non-uniform combination and easy migration of a long-afterglow luminescent material and a polyurethane coating and produce the light-storing luminescent coating with uniform color development and excellent glossiness and weather resistance.
A preparation method of a country experience type light-storing luminescent material comprises the following specific steps:
the method comprises the following steps: dehydrating the mixed solution of dihydric alcohol and trihydric alcohol for 3-5h at the temperature of 100-110 ℃ and under the vacuum condition of 0.05-0.2 MPa;
step two: adding an aliphatic ketone solution and an organotin solution into the dehydrated alcohol solution, mixing, heating to 70-80 ℃, adding triphenylmethane triisocyanate, and reacting at the temperature of 70-80 ℃ for 1.5-2.5 h;
step three: and (3) adding the light-storing luminescent material in the catalytic reaction, and continuing the heat preservation reaction to obtain the single-component light-storing polyurethane luminescent material.
The dihydric alcohol is one or two of polyether dihydric alcohol 2000 and polyester dihydric alcohol 2000.
The trihydric alcohol is one or two of polyether trihydric alcohol 3000 and polyester trihydric alcohol 3000.
The ketone solvent is one or two of acetone and butanone.
The organic tin solution is one or two of dibutyltin dilaurate and stannous octoate.
The light-storing luminescent material is red long afterglow luminescent material CaS, Eu and Dy.
The preparation method comprises the following specific steps:
the method comprises the following steps: mixing and adding 12-20 parts of polyether diol 2000 and 4-8 parts of polyether triol 3000 into a reactor, and dehydrating for 3.5-4.5h under the vacuum conditions of 103-108 ℃ and 0.05-0.2 MPa;
step two: adding 20-35 parts of acetone solution and 0.01-0.1 part of dibutyltin dilaurate solution into the dehydrated alcohol solution, mixing, heating to 70-78 ℃, adding 4-8 parts of triphenylmethane triisocyanate, and reacting at 70-78 ℃ for 1.5-2h under the condition of heat preservation;
step three: and 2-6 parts of light-storing luminescent material is added in the catalytic reaction, and the heat preservation reaction is continued for 0.8-1.8h to obtain the single-component light-storing polyurethane luminescent material.
The preparation method comprises the following specific steps:
the method comprises the following steps: mixing and adding 16 parts of polyether diol 2000 and 6 parts of polyether triol 3000 into a reactor, and dehydrating for 4 hours at 105 ℃ under the vacuum condition of 0.1 MPa;
step two: adding 30 parts of acetone solution and 0.01 part of dibutyltin dilaurate solution into the dehydrated alcohol solution, mixing, heating to 75 ℃, adding 6 parts of triphenylmethane triisocyanate, and reacting for 2 hours at 75 ℃ in a heat preservation manner;
step three: and after the NCO value in the solution reaches a theoretical value, adding 4 parts of red long-afterglow luminescent material CaS, Eu and Dy, and continuing to react for 1.5 hours under the condition of heat preservation to obtain the single-component light-storing polyurethane luminescent material.
The invention has the following beneficial effects:
(1) the country experience type light-storing luminescent material prepared by the polymerization reaction of the method not only has the excellent performance of a polyurethane material, but also increases the light-storing luminescent function of the coating, improves the problems of short chromophoric luminescent period, weak brightness, poor glossiness and weather resistance of the traditional fluorescent coating, obtains stable luminescence, is difficult to migrate, can keep the photophobic group stably for a long time, has excellent glossiness and weather resistance, is difficult to quench, increases the photophobic intensity, and displays the typical light-storing luminescent enhancement effect.
(2) According to the invention, through the ratio of the components, triphenyl methane triisocyanate reacts with other components to form a long-strip bone chain with a plurality of NCO branched chains uniformly distributed, the surface hydroxyl groups of the red long-afterglow luminescent inorganic material CaS, Eu and Dy can easily and respectively react with the NCO branched chains one by one, and then the CaS, Eu and Dy are completely connected with the NCO branched chains on the long-strip bone chain through radical reaction, as shown in the following formula 2:
therefore, a plurality of light-storing and light-emitting materials are regularly and continuously fixed on the whole long-strip bone chain, any NCO branched chain is not left for other reactions, and the stability of the long-strip bone chain can be ensured without end-capping treatment. Therefore, the luminous intensity is good in durability, stable in storage and not easy to quench, the distribution uniformity of the luminescent material particles is greatly improved, and the light absorption of the coating is uniform under the illumination condition, so that the coating achieves the effect of uniform and full luminescence, and the experience feeling is enhanced.
(3) According to the invention, through the proportion of each component, the reaction steps are simplified and the processing period is shortened on the premise of ensuring the excellent stability of the prepared single-component light-storing polyurethane luminescent material and improving the combination uniformity of the light-storing luminescent material and the polyurethane coating.
Drawings
The above and other features, advantages and aspects of various embodiments of the present disclosure will become more apparent by referring to the following detailed description when taken in conjunction with the accompanying drawings. In the drawings, like or similar reference numbers indicate like or similar items, and wherein:
FIG. 1 is a photograph comparing a polyurethane paint prepared by using diisocyanate (left A) and a country-experience type light-storing and light-emitting material prepared by the present invention (right B) coated on a wall surface.
FIG. 2 is a comparative graph of a polyurethane coating prepared using diisocyanate (left C) and a village-experienced light-storing and luminescent material prepared according to the present invention (right D) coated on a smooth plate, respectively, and displayed under an electron microscope.
FIG. 3 is a comparison of the night photographs of the polyurethane coating prepared by diisocyanate (left E) and the country-experience type light-storing and light-emitting material prepared by the present invention (right F) coated on the wall surface respectively.
Detailed Description
Example 1: a preparation method of a country experience type light-storing luminescent material comprises the following specific steps:
the method comprises the following steps: mixing and adding 16 parts of polyether diol 2000 and 6 parts of polyether triol 3000 into a reactor, and dehydrating for 4 hours at 105 ℃ under the vacuum condition of 0.1 MPa;
step two: adding 30 parts of acetone solution and 0.01 part of dibutyltin dilaurate solution into the dehydrated alcohol solution, mixing, heating to 75 ℃, adding 6 parts of triphenylmethane triisocyanate, and reacting for 2 hours at 75 ℃ in a heat preservation manner;
step three: and after the NCO value in the solution reaches a theoretical value, adding 4 parts of red long-afterglow luminescent material CaS, Eu and Dy, and continuing to react for 1.5 hours under the condition of heat preservation to obtain the single-component light-storing polyurethane luminescent material.
Example 2: a preparation method of a country experience type light-storing luminescent material comprises the following specific steps:
the method comprises the following steps: mixing and adding 12 parts of polyether diol 2000 and 4 parts of polyether triol 3000 into a reactor, and dehydrating for 3.5 hours at 103 ℃ under the vacuum condition of 0.05 MPa;
step two: adding 20 parts of acetone solution and 0.01 part of dibutyltin dilaurate solution into the dehydrated alcohol solution, mixing, heating to 70 ℃, adding 4 parts of triphenylmethane triisocyanate, and reacting for 1.5h at 70 ℃ in a heat preservation manner;
step three: 2 parts of red long-afterglow luminescent material CaS, Eu and Dy are added in the catalytic reaction, and the heat preservation reaction is continued for 0.8h to obtain the single-component light-storing polyurethane luminescent material.
Example 3: a preparation method of a country experience type light-storing luminescent material comprises the following specific steps:
the method comprises the following steps: mixing 20 parts of polyether diol 2000 and 8 parts of polyether triol 3000, adding into a reactor, and dehydrating for 4.5 hours at 108 ℃ under the vacuum condition of 0.2 MPa;
step two: adding 35 parts of acetone solution and 0.1 part of dibutyltin dilaurate solution into the dehydrated alcohol solution, mixing, heating to 78 ℃, adding 8 parts of triphenylmethane triisocyanate, and reacting for 2 hours at 78 ℃ in a heat preservation manner;
step three: 6 parts of red long-afterglow luminescent material CaS, Eu and Dy are added in the catalytic reaction, and the heat preservation reaction is continued for 1.8 hours to obtain the single-component light-storing polyurethane luminescent material.
Comparing the single-component light-storing polyurethane luminescent material prepared in the best embodiment 1 with a conventional luminescent polyurethane coating, as can be seen from fig. 1, the fluorescent polyurethane coating (left a) and the country-experience light-storing luminescent material (right B) prepared by the invention are respectively coated on the wall surface, and the difference between the fluorescent polyurethane coating (left a) and the country-experience light-storing luminescent material (right B) is not obvious after photographing under the conventional conditions.
The isocyanate and the polyol are gradually polymerized, and when the traditional diisocyanate or other isocyanates are used for reacting with the diol, the remaining NCO at the tail end of the reaction molecular chain reacts with the light-storing luminescent material for fixedly connecting the light-storing material, as shown in the following formula 1:
the light-storing luminescent material has small and unstable connecting amount, so that the prepared luminescent coating has weak brightness, unstable luminescent image, easy migration, poor persistence of the light-showing group and insufficient light-showing in the coating experience display process.
According to the invention, through the ratio of the components, triphenyl methane triisocyanate reacts with other components to form a long-strip skeleton chain with a plurality of NCO branched chains uniformly distributed, the surface hydroxyl groups of the red long-afterglow luminescent inorganic materials CaS, Eu and Dy can easily and respectively react with the NCO branched chains one by one, and the CaS, Eu and Dy are completely connected with the NCO branched chains on the long-strip skeleton chain through radical reaction, as shown in the following formula 2:
therefore, a plurality of light-storing and light-emitting materials are regularly and continuously fixed on the whole long-strip bone chain, any NCO branched chain is not left for other reactions, and the stability of the long-strip bone chain can be ensured without end-capping treatment. Therefore, the luminous intensity is good in durability, stable in storage and not easy to quench, the particles of the luminescent material are uniformly distributed, and the light absorption of the coating is uniform under the illumination condition, so that the coating achieves the effect of uniform and full luminescence, and the experience feeling is enhanced.
As can be seen from FIG. 2, under the electron microscope, the particles shown in the circle on the graph D are distinct and dense, i.e., the connected red long-afterglow luminescent inorganic materials CaS: Eu and Dy, while the particles in the graph C are not distinct and are relatively dispersed.
As can be seen from fig. 3, in the photograph taken at night, the written characters displayed in the F-diagram are obvious, the luminance is strong, and the light emission is stable, and the connection in the circle is continuous and obvious, while the characters displayed in the E-diagram are fuzzy, the luminance is poor, the light emission is unstable, and the connection in the circle is broken.
In order to make the objects, technical solutions and advantages of the embodiments of the present disclosure more clear, the technical solutions in the embodiments of the present disclosure are clearly and completely described, and it is obvious that the described embodiments are a part of the embodiments of the present disclosure, but 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.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (8)
1. A preparation method of a country experience type light-storing luminescent material is characterized in that: the method comprises the following specific steps:
the method comprises the following steps: dehydrating the mixed solution of dihydric alcohol and trihydric alcohol for 3-5h at the temperature of 100-110 ℃ and under the vacuum condition of 0.05-0.2 MPa;
step two: adding a ketone solvent and an organic tin catalyst into the dehydrated alcohol solution, mixing, heating to 70-80 ℃, adding triphenylmethane triisocyanate, and reacting for 1.5-2.5h at the temperature of 70-80 ℃;
step three: and (3) adding the light-storing luminescent material in the catalytic reaction, and continuing the heat preservation reaction to obtain the single-component light-storing polyurethane luminescent material.
2. The method for preparing a village experience type light-storing luminescent material as claimed in claim 1, wherein said method comprises the steps of: the dihydric alcohol is one or two of polyether dihydric alcohol 2000 and polyester dihydric alcohol 2000.
3. The method for preparing a village experience type light-storing luminescent material as claimed in claim 1, wherein said method comprises the steps of: the trihydric alcohol is one or two of polyether trihydric alcohol 3000 and polyester trihydric alcohol 3000.
4. The method for preparing a village experience type light-storing luminescent material as claimed in claim 1, wherein said method comprises the steps of: the ketone solvent is one or two of acetone and butanone.
5. The method for preparing a village experience type light-storing luminescent material as claimed in claim 1, wherein said method comprises the steps of: the organic tin solution is one or two of dibutyltin dilaurate and stannous octoate.
6. The method for preparing a village experience type light-storing luminescent material as claimed in claim 1, wherein said method comprises the steps of: the light-storing luminescent material is red long afterglow luminescent material CaS, Eu and Dy.
7. The method for preparing a village experience type light-storing luminescent material as claimed in claim 1, wherein said method comprises the steps of: the method comprises the following specific steps:
the method comprises the following steps: mixing and adding 12-20 parts of polyether diol 2000 and 4-8 parts of polyether triol 3000 into a reactor, and dehydrating for 3.5-4.5h under the vacuum conditions of 103-108 ℃ and 0.05-0.2 MPa;
step two: adding 20-35 parts of acetone solution and 0.01-0.1 part of dibutyltin dilaurate solution into the dehydrated alcohol solution, mixing, heating to 70-78 ℃, adding 4-8 parts of triphenylmethane triisocyanate, and reacting at 70-78 ℃ for 1.5-2h under the condition of heat preservation;
step three: and 2-6 parts of light-storing luminescent material is added in the catalytic reaction, and the heat preservation reaction is continued for 0.8-1.8h to obtain the single-component light-storing polyurethane luminescent material.
8. The method for preparing a village experience type light-storing luminescent material as claimed in claim 1, wherein said method comprises the steps of: the preparation method comprises the following specific steps:
the method comprises the following steps: mixing and adding 16 parts of polyether diol 2000 and 6 parts of polyether triol 3000 into a reactor, and dehydrating for 4 hours at 105 ℃ under the vacuum condition of 0.1 MPa;
step two: adding 30 parts of acetone solution and 0.01 part of dibutyltin dilaurate solution into the dehydrated alcohol solution, mixing, heating to 75 ℃, adding 6 parts of triphenylmethane triisocyanate, and reacting for 2 hours at 75 ℃ in a heat preservation manner;
step three: and after the NCO value in the solution reaches a theoretical value, adding 4 parts of red long-afterglow luminescent material CaS, Eu and Dy, and continuing to react for 1.5 hours under the condition of heat preservation to obtain the single-component light-storing polyurethane luminescent material.
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