CN112342015B - High-brightness fluorescent magnetic powder, preparation method thereof and high-brightness fluorescent magnetic powder concentrated solution - Google Patents
High-brightness fluorescent magnetic powder, preparation method thereof and high-brightness fluorescent magnetic powder concentrated solution Download PDFInfo
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- CN112342015B CN112342015B CN201910725831.8A CN201910725831A CN112342015B CN 112342015 B CN112342015 B CN 112342015B CN 201910725831 A CN201910725831 A CN 201910725831A CN 112342015 B CN112342015 B CN 112342015B
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Abstract
The invention discloses high-brightness fluorescent magnetic powder which is prepared by grafting fluorescein with active functional groups onto the surface of surface-functionalized low-brightness fluorescent magnetic powder; the surface functionalized low-brightness fluorescent magnetic powder is prepared by mixing and reacting a hybrid reagent, magnetic powder and fluorescent powder. The invention has simple production process and lower cost, can graft various active fluorescein on the surface of the low-brightness fluorescent magnetic powder, improves the fluorescent brightness of the fluorescent magnetic powder and improves the sensitivity of the fluorescent magnetic powder.
Description
Technical Field
The invention relates to the technical field of preparation of high-brightness fluorescent magnetic powder, in particular to high-brightness fluorescent magnetic powder, a preparation method thereof and a high-brightness fluorescent magnetic powder concentrated solution.
Background
The fluorescent magnetic powder takes an important role in the field of magnetic nondestructive inspection, is prepared by taking a magnetic material as a core and adhering a layer of fluorescent dye on the outer surface of the core by using epoxy resin through a physical or chemical method, and under the irradiation of ultraviolet light, fluorescence generated by the magnetic powder has a sharp contrast with a workpiece, so that the existence of the workpiece defect is easier to observe.
However, the traditional fluorescent magnetic powder has low fluorescent brightness, which greatly affects the sensitivity of the fluorescent magnetic powder and easily causes missing detection to reduce the safety factor of the product. The adhesion amount of the fluorescent magnetic powder is increased, the brightness of the fluorescent magnetic powder can be effectively improved, but the particle size of the fluorescent magnetic powder is increased easily, and the magnetic responsivity of the fluorescent magnetic powder is reduced easily.
Disclosure of Invention
The invention aims to provide high-brightness fluorescent magnetic powder, a preparation method thereof and a fluorescent magnetic powder concentrated solution, aiming at overcoming the technical defects.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect of the present invention, there is provided a high-brightness fluorescent magnetic powder prepared by grafting fluorescein having an active functional group onto the surface of a surface-functionalized low-brightness fluorescent magnetic powder; the surface functionalized low-brightness fluorescent magnetic powder is prepared by mixing and reacting a hybrid reagent, magnetic powder and fluorescent powder.
Preferably, the hybridization reagent comprises the following components in parts by mass: 5-10 parts of reactive compound, 85-95 parts of adhesive and 1-5 parts of curing agent.
Preferably, the reactive compound is an alkyl polyamine or an alkyl carboxylic acid.
Preferably, the reactive functional group on the fluorescein is an isothiocyanate, a carboxyl group or an amine group.
Preferably, the magnetic powder is carbonyl iron powder, ferric oxide, ferroferric oxide or cobalt powder.
In a second aspect of the present invention, a method for preparing the above high brightness fluorescent magnetic powder is provided, which includes the following steps:
s1, putting 5-10 parts of reactive compound, 85-95 parts of adhesive and 1-5 parts of curing agent into a stirring container, and stirring and mixing uniformly to obtain a hybrid reagent;
s2, adding 2-5 parts of the hybrid reagent prepared in the step S1, 80-90 parts of magnetic powder and 20-30 parts of fluorescent powder into another stirring container, heating to 120 ℃, stirring for reaction for 30min, and then drying, crushing and sieving to obtain surface functionalized low-brightness fluorescent magnetic powder;
s3, dispersing 92-97 parts of the surface functionalized low-brightness fluorescent magnetic powder prepared in the step S2 and 3-8 parts of fluorescein with active functional groups in an aqueous solution, stirring and reacting, and adsorbing the reacted fluorescent magnetic powder by a magnet to obtain the high-brightness fluorescent magnetic powder.
In a third aspect of the present invention, a high-brightness fluorescent magnetic powder concentrated solution is provided, which includes high-brightness fluorescent magnetic powder.
Preferably, the high-brightness fluorescent magnetic powder concentrated solution comprises the following components in parts by mass: 80-100 parts of high-brightness fluorescent magnetic powder, 10-20 parts of defoaming agent, 10-20 parts of dispersing agent, 50-70 parts of antirust agent and 300 parts of water 250-.
Preferably, the defoaming agent is an organic silicon defoaming agent, the dispersing agent is sodium dodecyl benzene sulfonate, and the antirust agent is triethanolamine.
Compared with the prior art, the invention has the following beneficial effects:
the high-brightness fluorescent magnetic powder prepared by the invention is a micron hybrid material, and is prepared by dispersing a reactive compound in an adhesive layer, hybridizing functional groups such as amino or carboxyl and the like onto the surface of the low-brightness fluorescent magnetic powder, and grafting fluorescein with corresponding active functional groups onto the surface of the fluorescent magnetic powder, so that the brightness of the fluorescent magnetic powder is improved, the particle size of the fluorescent magnetic powder is not increased, and the magnetic responsiveness is still high. Compared with the prior fluorescent magnetic powder, the high-brightness fluorescent magnetic powder concentrated solution prepared by the invention greatly reduces the use amount when in use. The production process of the high-brightness fluorescent magnetic powder is simple, the cost is low, multiple fluorescein can be grafted to the surface of the low-brightness fluorescent magnetic powder, the fluorescent brightness is obviously improved, the magnetic powder particles are still fine, the sensitivity is greatly improved, the magnetic damage detection leakage rate is greatly reduced, the quality and the safety performance of the product are obviously improved, and the method has an important social effect.
Drawings
The invention is described in further detail below with reference to specific embodiments and with reference to the following drawings.
FIG. 1 is a TEM image of the high brightness fluorescent magnetic powder concentrated solution and the conventional fluorescent magnetic powder on A1 test piece in example 4;
FIG. 2 is a TEM image of the high brightness fluorescent magnetic powder concentrated solution and the conventional fluorescent magnetic powder on a type I test block in example 4;
FIG. 3 is a graph showing the comparison of the fluorescent brightness of the high-brightness fluorescent magnetic powder concentrated solution and the conventional fluorescent magnetic powder in example 4;
FIG. 4 is a schematic view showing the reaction of the surface-functionalized low-brightness fluorescent magnetic powder with fluorescein having isothiocyanate functional group in example 1;
FIG. 5 is a schematic view showing the reaction between the surface-functionalized low-brightness fluorescent magnetic powder and the amine-group-containing fluorescein in example 3.
Detailed Description
Example 1
The embodiment provides high-brightness fluorescent magnetic powder, which is prepared by the following steps:
s1, putting 50g of reactive compound (selected from alkyl polyamine, R-NH2), 920g of adhesive (selected from epoxy resin emulsion) and 30g of curing agent (polyamide) into a stirring container, and stirring at high speed to mix uniformly to obtain a hybrid reagent;
s2, adding 300g of the hybridization reagent prepared in the step S1, 8kg of magnetic powder (carbonyl iron powder is selected) and 2kg of fluorescent powder into another stirring container, heating to 120 ℃, stirring for reaction for 30min, then placing the mixture into an oven for drying treatment at 200 ℃ for 1h, crushing the mixture, and sieving the crushed mixture through a 300-350-mesh sieve to obtain surface functionalized low-brightness fluorescent magnetic powder;
s3, dispersing 920g of the surface functionalized low-brightness fluorescent magnetic powder prepared in the step S2 and 80g of fluorescein with isothiocyanate functional groups (selected from fluorescein isothiocyanate, FITC) in an aqueous solution, stirring for reaction, and adsorbing the reacted fluorescent magnetic powder by a magnet to obtain the high-brightness fluorescent magnetic powder, wherein the reaction schematic diagram is shown in figure 4.
The chemical reaction of fluorescein isothiocyanate and amine on the surface of fluorescent magnetic powder is as follows:
the fluorescein is grafted to the surface of the low-brightness fluorescent magnetic powder through the reaction, so that the aim of brightening the fluorescent magnetic powder is fulfilled.
Example 2
The embodiment provides high-brightness fluorescent magnetic powder, which is prepared by the following steps:
s1, putting 70g of reactive compound (selected from alkyl polyamine, R-NH2), 850g of adhesive (selected from epoxy resin emulsion) and 10g of curing agent (polyamide) into a stirring container, and stirring at high speed to mix uniformly to obtain a hybrid reagent;
s2, adding 500g of the hybrid reagent prepared in the step S1, 8.6kg of magnetic powder (carbonyl iron powder is selected) and 2.3kg of fluorescent powder into another stirring container, heating to 120 ℃, stirring for reaction for 30min, then placing the mixture into an oven, drying for 1h at 200 ℃, crushing, and sieving with a 300-fold 350-mesh sieve to obtain surface functionalized low-brightness fluorescent magnetic powder;
s3, dispersing 970g of the surface functionalized low-brightness fluorescent magnetic powder prepared in the step S2 and 30g of fluorescein with active carboxyl functional groups in an aqueous solution, stirring for reaction, and adsorbing the reacted fluorescent magnetic powder by using a magnet to obtain the high-brightness fluorescent magnetic powder.
Wherein, the chemical reaction of the carboxylated fluorescein and the amine on the surface of the fluorescent magnetic powder is as follows:
example 3
The embodiment provides high-brightness fluorescent magnetic powder, which is prepared by the following steps:
s1, putting 100g of reactive active compound (alkyl carboxylic acid, R-COOH) selected, 950g of adhesive (epoxy resin emulsion selected) and 50g of curing agent (polyamide) into a stirring container, and stirring at high speed to mix uniformly to obtain a hybrid reagent;
s2, adding 200g of the hybrid reagent prepared in the step S1, 9kg of magnetic powder (carbonyl iron powder is selected) and 3kg of fluorescent powder into another stirring container, heating to 120 ℃, stirring for reaction for 30min, then placing the mixture into an oven, drying the mixture for 1h at 200 ℃, crushing the mixture, and sieving the crushed mixture through a 300-fold 350-mesh sieve to obtain surface functionalized low-brightness fluorescent magnetic powder;
s3, dispersing 940g of the surface functionalized low-brightness fluorescent magnetic powder prepared in the step S2 and 60g of fluorescein (rhodamine is selected) with amido into the water solution, stirring and reacting, and adsorbing the reacted fluorescent magnetic powder by a magnet to obtain the high-brightness fluorescent magnetic powder, wherein the reaction schematic diagram is shown in FIG. 5.
Wherein, the chemical reaction of the carboxyl hybridized low-brightness fluorescent magnetic powder and the amino group-containing fluorescein (such as rhodamine) is as follows:
example 4
This example provides a high-brightness fluorescent magnetic powder concentrated solution, which is prepared by sequentially adding 80g of the high-brightness fluorescent magnetic powder prepared in example 1, 10g of a dispersant (sodium dodecyl benzene sulfonate), 20g of an organic silicon defoamer, and 70g of a rust inhibitor triethanolamine into 250g of water, and uniformly mixing the mixture at a low speed.
Example 5
This example provides a high-brightness fluorescent magnetic powder concentrated solution, which is prepared by sequentially adding 92g of the high-brightness fluorescent magnetic powder prepared in example 1, 16g of a dispersant (sodium dodecyl benzene sulfonate), 10g of an organic silicon defoamer, and 50g of a rust inhibitor triethanolamine into 260g of water, and uniformly stirring and mixing at a low speed.
Example 6
This example provides a high-brightness fluorescent magnetic powder concentrated solution, which is prepared by sequentially adding 100g of the high-brightness fluorescent magnetic powder prepared in example 1, 20g of a dispersant (sodium dodecyl benzene sulfonate), 14g of an organic silicon defoamer and 61g of an antirust triethanolamine into 300g of water, and uniformly stirring and mixing at a low speed.
Test examples
The high-brightness fluorescent magnetic powder concentrated solution prepared in example 4 and the conventional fluorescent magnetic powder were dispersed in water, respectively, to prepare a magnetic suspension containing 1g of fluorescent magnetic powder per liter of water, and the properties of the two were measured, and the measurement results are shown in table 1.
TABLE 1
As shown in table 1 and fig. 1 to 3, the fluorescent magnetic powder of the present invention has higher fluorescent brightness and higher sensitivity than the conventional fluorescent magnetic powder, which is beneficial to preventing the omission of the critical workpiece and improving the safety performance of the product.
The present invention has been described in terms of specific examples, which are provided to aid understanding of the invention and are not intended to be limiting. Numerous simple deductions, modifications or substitutions may also be made by those skilled in the art in light of the present teachings.
Claims (7)
1. The high-brightness fluorescent magnetic powder is characterized in that the high-brightness fluorescent magnetic powder is prepared by grafting fluorescein with active functional groups onto the surface of surface-functionalized low-brightness fluorescent magnetic powder; the surface functionalized low-brightness fluorescent magnetic powder is prepared by mixing and reacting a hybridization reagent, magnetic powder and fluorescent powder;
the hybridization reagent comprises the following components in parts by mass: 5-10 parts of reactive compound, 85-95 parts of adhesive and 1-5 parts of curing agent;
the reactive compound is an alkyl polyamine or an alkyl carboxylic acid.
2. The high brightness fluorescent magnetic powder of claim 1, wherein the reactive functional group on fluorescein is isothiocyanate, carboxyl or amine.
3. A high brightness fluorescent magnetic powder according to claim 1, wherein said powder is carbonyl iron powder, iron sesquioxide, iron tetroxide or cobalt powder.
4. A method for preparing the high brightness fluorescent magnetic powder according to claim 2, comprising the steps of:
s1, putting 5-10 parts of reactive compound, 85-95 parts of adhesive and 1-5 parts of curing agent into a stirring container, and stirring and mixing uniformly to obtain a hybrid reagent;
s2, adding 2-5 parts of the hybrid reagent prepared in the step S1, 80-90 parts of magnetic powder and 20-30 parts of fluorescent powder into another stirring container, heating to 120 ℃, stirring for reaction for 30min, and then drying, crushing and sieving to obtain surface functionalized low-brightness fluorescent magnetic powder;
s3, dispersing 92-97 parts of the surface functionalized low-brightness fluorescent magnetic powder prepared in the step S2 and 3-8 parts of fluorescein with active functional groups in an aqueous solution, stirring and reacting, and adsorbing the reacted fluorescent magnetic powder by a magnet to obtain the high-brightness fluorescent magnetic powder.
5. A high-brightness fluorescent magnetic powder concentrated solution, characterized in that the high-brightness fluorescent magnetic powder concentrated solution comprises the high-brightness fluorescent magnetic powder according to any one of claims 1 to 3.
6. The high-brightness fluorescent magnetic powder concentrated solution according to claim 5, comprising the following components in parts by mass: 80-100 parts of high-brightness fluorescent magnetic powder, 10-20 parts of defoaming agent, 10-20 parts of dispersing agent, 50-70 parts of antirust agent and 300 parts of water 250-.
7. The high-brightness fluorescent magnetic powder concentrate as recited in claim 6, wherein the defoamer is an organic silicon defoamer, the dispersant is sodium dodecyl benzene sulfonate, and the rust inhibitor is triethanolamine.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3485758A (en) * | 1967-06-27 | 1969-12-23 | Magnaflux Corp | Method of making fluorescent magnetic particles |
| US4576912A (en) * | 1978-11-30 | 1986-03-18 | Technicon Instruments Corporation | Fluoroimmunoassaying |
| US4724094A (en) * | 1985-02-07 | 1988-02-09 | Magnaflux Corporation | Fluorescent magnetic composition and method of making and using same |
| CN105936820A (en) * | 2016-04-20 | 2016-09-14 | 北京工商大学 | Water soluble biocompatible fluorescent magnetic nanoclusters and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009227761A (en) * | 2008-03-21 | 2009-10-08 | Fuji Xerox Co Ltd | Fluorescent magnetic powder, method for producing the same, magnetic ink composition, magnetic polymer particles, liquid developer for magnetic latent image, cartridge and image forming apparatus |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3485758A (en) * | 1967-06-27 | 1969-12-23 | Magnaflux Corp | Method of making fluorescent magnetic particles |
| GB1177703A (en) * | 1967-06-27 | 1970-01-14 | Magnaflux Corp | Improvements in or relating to Flourescent Magnetic Particles |
| US4576912A (en) * | 1978-11-30 | 1986-03-18 | Technicon Instruments Corporation | Fluoroimmunoassaying |
| US4724094A (en) * | 1985-02-07 | 1988-02-09 | Magnaflux Corporation | Fluorescent magnetic composition and method of making and using same |
| CN105936820A (en) * | 2016-04-20 | 2016-09-14 | 北京工商大学 | Water soluble biocompatible fluorescent magnetic nanoclusters and preparation method thereof |
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