CN111257408A - Effervescent tablet containing nano magnetic powder and application thereof - Google Patents

Effervescent tablet containing nano magnetic powder and application thereof Download PDF

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Publication number
CN111257408A
CN111257408A CN202010099838.6A CN202010099838A CN111257408A CN 111257408 A CN111257408 A CN 111257408A CN 202010099838 A CN202010099838 A CN 202010099838A CN 111257408 A CN111257408 A CN 111257408A
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effervescent tablet
magnetic powder
forming agent
nano
agent
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CN111257408B (en
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王玉亮
詹超
杨新健
黄桂林
孔令昌
李欢
李青松
孙吉
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Guangdong Inspection and Research Institute of Special Equipment Zhuhai Inspection Institute
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Guangdong Inspection and Research Institute of Special Equipment Zhuhai Inspection Institute
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/72Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating magnetic variables
    • G01N27/82Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating magnetic variables for investigating the presence of flaws
    • G01N27/83Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating magnetic variables for investigating the presence of flaws by investigating stray magnetic fields
    • G01N27/84Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating magnetic variables for investigating the presence of flaws by investigating stray magnetic fields by applying magnetic powder or magnetic ink
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/0302Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity characterised by unspecified or heterogeneous hardness or specially adapted for magnetic hardness transitions
    • H01F1/0311Compounds
    • H01F1/0313Oxidic compounds
    • H01F1/0315Ferrites

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Abstract

The invention belongs to the technical field of detection, and discloses an effervescent tablet containing nano magnetic powder, which comprises the following components: nano magnetic powder, a dispersing agent, a defoaming agent, a forming agent, alkaline carbonate and a film-forming agent; the nanometer magnetic powder is nanometer Fe2O3. The nanometer magnetic powder in the effervescent tablet is simultaneously used with the polyoxyethylene polyoxypropylene block copolymer, the triethanolamine or the sodium benzoate, so that the effervescent tablet is mixed with water to prepare the water magnetic suspension, the nanometer magnetic powder in the water magnetic suspension can be uniformly and stably dispersed, and the detection sensitivity can be improved. The nanometer magnetic powder used by the effervescent tablet is nanometer gamma-Fe2O3Nano gamma-Fe2O3The prepared effervescent tablet is red, when the effervescent tablet is used for detecting workpiece damage, auxiliary spraying of a contrast toner is not needed, the effervescent tablet is convenient to use, the detection cost is reduced, the width of a crack which can be detected can reach 0.1 micrometer, the length of the crack can reach 0.5 micrometer, and the detection sensitivity is high. The effervescent tablet of the invention can be prepared into solidThe tablets with fixed specification and quality are convenient to use and transport.

Description

Effervescent tablet containing nano magnetic powder and application thereof
Technical Field
The invention belongs to the technical field of detection, and particularly relates to an effervescent tablet containing nano magnetic powder and application thereof.
Background
The nondestructive inspection is to inspect the structure, property and state of the inner part and surface of an object to be inspected (such as a metal workpiece) with high sensitivity and high reliability without damaging or changing the physical and chemical state of the object, so as to obtain the integrity, safety and other performance indexes of the object to be inspected. Magnetic particle inspection is a method for detecting defects in a workpiece by utilizing a magnetic phenomenon, is a nondestructive detection method, is usually used for finding defects on the surface and near the surface of a ferromagnetic material or the workpiece, and is suitable for detecting defects which are small in surface size, narrow in gap (for example, cracks with the width of 0.1mm and the length of 10 microns can be detected) and difficult to see visually, such as cracks, white spots, hairlines, folds, looseness, cold shut, air holes, slag inclusions and the like. Martensitic stainless steel and precipitation hardening stainless steel materials (such as 1Cr17Ni7) are magnetic and therefore can also be subjected to magnetic particle inspection.
At present, in the nondestructive inspection industry, magnetic paste or magnetic powder and reagents such as wetting agents, dispersing agents, preservatives and the like are generally adopted to prepare the hydromagnetic suspension on site, and then workpieces are detected. In addition, the sensitivity of the workpiece detected by using the magnetic paste or magnetic powder to prepare the water-magnetic suspension on site can only reach the sensitivity of cracks with the length of 0.1mm and the width of 10 microns generally, and the crack can not be detected for finer cracks. In addition, the storage stability of the magnetic paste or the magnetic powder under the conventional conditions is poor, and the transportation is inconvenient. In particular, in the prior art, magnetic paste or magnetic powder is used for detecting the surface of a workpiece, a contrast enhancer is usually sprayed on the surface of the workpiece (the contrast enhancer has the function of highlighting the difference between the color of the magnetic powder of the effervescent tablet and the color of the workpiece, and is beneficial to a magnetic detector to read crack data on the surface of the workpiece), and the main component of the commonly used contrast enhancer is a mixture of acetone and zinc oxide. Spraying contrast enhancers is beneficial to improving the sensitivity of detection, but makes the detection process cumbersome and also increases the detection cost.
Accordingly, it is desirable to provide a magnetic detection material that has high detection sensitivity, good stability, no need for a contrast enhancer for auxiliary use, and convenient transportation.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art described above. Therefore, the invention provides an effervescent tablet containing nano magnetic powder and application thereof. The effervescent tablet containing the magnetic powder has high sensitivity of detecting workpieces and good stability, and does not need a contrast enhancer for auxiliary use.
An effervescent tablet containing nanometer magnetic powder comprises the following components: nano magnetic powder, a dispersing agent, a defoaming agent, a forming agent, alkaline carbonate and a film-forming agent; the nanometer magnetic powder is nanometer Fe2O3
Preferably, the nano Fe2O3Is nano gamma-Fe2O3. Nano gamma-Fe2O3The prepared effervescent tablet is red, when the effervescent tablet is used for detecting workpiece damage, auxiliary spraying of a contrast toner is not needed, the use is convenient, the detection cost is reduced, and the detection sensitivity is high.
Preferably, the particle size of the nanometer magnetic powder is 1-100 nm; further preferably, the particle size of the nanometer magnetic powder is 30-50 nm.
Preferably, the dispersant is selected from at least one of polyoxyethylene polyoxypropylene block copolymer, triethanolamine or sodium benzoate; further preferably, the nitrite is sodium nitrite. The dispersing agent has the function that when the effervescent tablets are mixed with water to prepare the water magnetic suspension, the nano magnetic powder in the water magnetic suspension can be uniformly and stably dispersed, and the detection sensitivity can be improved.
Preferably, the defoaming agent is nano silicon dioxide.
Preferably, the forming agent is at least one of sodium chloride, potassium chloride or magnesium chloride.
Preferably, the alkaline carbonate is at least one of sodium carbonate, potassium carbonate, sodium bicarbonate or potassium bicarbonate; more preferably, the alkali carbonate is sodium bicarbonate. The alkaline carbonate salt causes the effervescent tablet to disintegrate rapidly in water.
Preferably, the film forming agent is a pyrrolidone substance, and further preferably, the film forming agent is polyvinylpyrrolidone. The film forming agent can form an excellent continuous coating film, is beneficial to wetting and dispersing magnetic powder and is beneficial to forming a stable effervescent tablet.
Preferably, the effervescent tablet further comprises a sulfate; further preferably, the sulfate is magnesium sulfate; is helpful for improving the stability of the effervescent tablet.
Preferably, the effervescent tablet also contains trichloroisocyanuric acid.
Preferably, the effervescent tablet containing the nanometer magnetic powder comprises the following components in percentage by mass: 20-35% of nano magnetic powder, 30-40% of dispersing agent, 1-3% of defoaming agent, 5-15% of forming agent, 3-7% of alkaline carbonate and the balance of film-forming agent.
Further preferably, the effervescent tablet containing the nanometer magnetic powder comprises the following components in percentage by mass: 25% of nano magnetic powder, 13% of polyoxyethylene polyoxypropylene block copolymer, 7% of triethanolamine, 12% of sodium benzoate, 3% of defoaming agent, 10% of forming agent, 5% of alkaline carbonate, 2% of film-forming agent, 15% of magnesium sulfate and 8% of trichloroisocyanuric acid.
More preferably, the effervescent tablet containing the magnetic powder comprises the following components in percentage by mass: 20% of nano magnetic powder, 14% of polyoxyethylene polyoxypropylene block copolymer, 8% of triethanolamine, 13% of sodium benzoate, 3% of defoaming agent, 10% of forming agent, 7% of alkaline carbonate, 2% of film-forming agent, 15% of magnesium sulfate and 8% of trichloroisocyanuric acid.
A method for preparing effervescent tablet containing nanometer magnetic powder comprises the following steps:
weighing the components, mixing the magnetic powder with the film-forming agent, then adding the other components except the forming agent, stirring and mixing uniformly, then adding the forming agent, stirring and mixing uniformly, and tabletting for forming to obtain the effervescent tablet containing the magnetic powder.
Preferably, the film-forming agent is mixed with water to prepare a solution with the mass concentration of 8-12%, and then the solution is mixed with the nano magnetic powder.
Preferably, the magnetic powder is mixed with the film-forming agent and then dried, wherein the drying is carried out for 3 to 5 hours at a temperature of between 50 and 80 ℃.
Preferably, the water content of each raw material is less than 1% (mass fraction).
Preferably, the tablet forming process is maintained at a pressure of 20-50KN for 1-60 seconds.
Preferably, the whole process for preparing the effervescent tablet is carried out under the conditions that the temperature is 18-25 ℃ and the relative humidity is not more than 40%. Is favorable for preventing the effervescent tablets from being affected with damp.
Preferably, the effervescent tablet has a mass specification of 1g, 2g, 5g, 8g, 10g, 20g, 40g or 50 g.
A use method of an effervescent tablet containing nanometer magnetic powder comprises the following steps:
mixing effervescent tablet with water to form water magnetic suspension, spraying onto workpiece surface, magnetizing the workpiece surface with magnetic detector, and detecting the defect data of the workpiece surface.
Preferably, the dosage ratio of the effervescent tablets to water is 40-80g: 1L; further preferably, the dosage ratio of the effervescent tablets to the water is 60g to 1L.
Preferably, the workpiece is a ferromagnetic metal workpiece.
Preferably, the pH of the mixture of the effervescent tablets dissolved in water is 3-6.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the effervescent tablet, the nanometer magnetic powder and the dispersing agent are mixed for use, particularly the magnetic powder is simultaneously used with the polyoxyethylene polyoxypropylene block copolymer, the triethanolamine or the sodium benzoate, so that the effervescent tablet is mixed with water to prepare the water magnetic suspension, the nanometer magnetic powder in the water magnetic suspension can be uniformly and stably dispersed, and the detection sensitivity can be improved.
(2) The nano magnetic powder used by the effervescent tablet is nano gamma-Fe2O3Nano gamma-Fe2O3The prepared effervescent tablet is red, when the effervescent tablet is used for detecting workpiece damage, auxiliary spraying of a contrast toner is not needed, the use is convenient, the detection cost is reduced, and the detection sensitivity is high.
(3) The effervescent tablet is used for detecting defects on the surface and near surface of a workpiece, and can detect cracks with the width of 0.1 mu m and the length of 0.5 mu m, and the detection sensitivity is high.
(4) The effervescent tablet can be prepared into tablets with fixed specification and quality, and is convenient to use and transport.
Detailed Description
In order to make the technical solutions of the present invention more apparent to those skilled in the art, the following examples are given for illustration. It should be noted that the following examples are not intended to limit the scope of the claimed invention.
The starting materials, reagents or apparatuses used in the following examples are conventionally commercially available or can be obtained by conventionally known methods, unless otherwise specified.
Example 1
An effervescent tablet containing nano magnetic powder comprises the following components in percentage by mass: 20-30nm Fe2O325g, 13g of polyoxyethylene polyoxypropylene block copolymer, 7g of triethanolamine, 12g of sodium benzoate, 3g of nano silicon dioxide, 10g of sodium chloride, 5g of sodium carbonate, 2g of polyvinylpyrrolidone, 15g of magnesium sulfate and 8g of trichloroisocyanuric acid.
A method for preparing effervescent tablet containing nanometer magnetic powder comprises the following steps:
weighing the components, mixing polyvinylpyrrolidone with water to prepare a solution with the mass concentration of 9%, and then adding Fe2O3Mixing, oven drying at 60 deg.C for 4 hr, adding the rest components except sodium chloride, stirring, mixing, and addingAdding sodium chloride, stirring, mixing, tabletting under 40KN for 30 s to obtain effervescent tablet containing nanometer magnetic powder.
The whole preparation process of the effervescent tablet is carried out under the conditions that the temperature is 20 ℃ and the relative humidity is 30 percent.
Example 2
An effervescent tablet containing nano magnetic powder comprises the following components in percentage by mass: 30-50nm gamma-Fe2O320g, 14g of polyoxyethylene polyoxypropylene block copolymer, 8g of triethanolamine, 13g of sodium benzoate, 3g of nano silicon dioxide, 10g of potassium chloride, 7g of alkaline carbonate, 2g of polyvinylpyrrolidone, 15g of magnesium sulfate and 8g of trichloroisocyanuric acid.
A method for preparing effervescent tablet containing nanometer magnetic powder comprises the following steps:
weighing the components, mixing polyvinylpyrrolidone with water to prepare a solution with the mass concentration of 12%, and then adding gamma-Fe2O3And drying at 80 ℃ for 3.5 hours, adding the other components except the potassium chloride, stirring and mixing uniformly, adding the potassium chloride, stirring and mixing uniformly, tabletting and forming, wherein the tabletting and forming process is to keep the pressure at 50KN for 40 seconds, and thus the effervescent tablet containing the nano magnetic powder is prepared.
The whole preparation process of the effervescent tablet is carried out under the conditions that the temperature is 25 ℃ and the relative humidity is 25 percent.
Example 3
An effervescent tablet containing nano magnetic powder comprises the following components in percentage by mass: 40-60nm gamma-Fe2O335g, 16g of polyoxyethylene polyoxypropylene block copolymer, 20g of sodium benzoate, 2g of nano silicon dioxide, 9g of sodium chloride, 7g of sodium bicarbonate and 11g of polyvinylpyrrolidone.
A method for preparing effervescent tablet containing nanometer magnetic powder comprises the following steps:
weighing the components, mixing polyvinylpyrrolidone with water to prepare a solution with the mass concentration of 6%, and then adding gamma-Fe2O3Drying at 65 deg.C for 3.5 hr, addingAdding the rest components except sodium chloride, stirring, mixing, adding sodium chloride, stirring, mixing, tabletting under 40KN for 60 s to obtain effervescent tablet containing nanometer magnetic powder.
The whole preparation process of the effervescent tablet is carried out under the conditions that the temperature is 20 ℃ and the relative humidity is 30 percent.
Example 4
An effervescent tablet containing nano magnetic powder comprises the following components in percentage by mass: 40-60nm Fe2O332g, 15g of polyoxyethylene polyoxypropylene block copolymer, 15g of triethanolamine, 3g of nano silicon dioxide, 12g of potassium chloride, 10g of potassium carbonate and 13g of polyvinylpyrrolidone.
A preparation method of effervescent tablets containing magnetic powder comprises the following steps:
weighing the components, mixing polyvinylpyrrolidone with water to prepare a solution with the mass concentration of 8%, and then adding Fe3O4And drying at 70 ℃ for 3 hours, adding the other components except the potassium chloride, stirring and mixing uniformly, adding the potassium chloride, stirring and mixing uniformly, tabletting and forming, wherein the tabletting and forming process is to keep the pressure at 45KN for 50 seconds, and preparing the effervescent tablet containing the nano magnetic powder.
Comparative example 1
In comparison with example 2, comparative example 1 does not contain polyoxyethylene polyoxypropylene block copolymer, triethanolamine or sodium benzoate, and the rest of the components and preparation method are the same as example 2.
Product effectiveness testing
The effervescent tablets prepared in examples 1 to 4 and comparative example 1 were mixed according to the amount ratio of the effervescent tablet to water of 60g:1L to prepare an aqueous magnetic suspension, and after observing the disintegration time of the effervescent tablet in water and then standing at 20 ℃ for 2 hours, the dispersion of the aqueous magnetic suspension was observed to see whether or not a precipitate appeared and also the defoaming was observed, and the results are shown in Table 1.
Table 1:
disintegration time (minutes) Dispersion situation Defoaming conditions
Example 1 8.4 No precipitation Non-foam
Example 2 8.2 No precipitation Non-foam
Example 3 8.3 No precipitation Non-foam
Example 4 8.5 No precipitation Non-foam
Comparative example 1 8.5 A little precipitate Little foam
As can be seen from Table 1, the dispersion and defoaming of the effervescent tablets prepared in examples 1 to 4 of the present invention are significantly better than those of the effervescent tablet prepared in comparative example 1.
The effervescent tablets prepared in examples 1 to 4 and comparative example 1 were respectively placed in an electric-heating constant-humidity constant-temperature incubator at 40. + -. 2 ℃ and a relative humidity of 50. + -. 10% for 6 months, and then tested for the mass change rate of magnetic powder, and the results are shown in Table 2.
Table 2:
Figure BDA0002386582610000061
as can be seen from Table 2, the effervescent tablets prepared in examples 1 to 4 of the present invention have good stability in the solid state, and are convenient for storage and transportation.
Example 5
A use method of an effervescent tablet containing nanometer magnetic powder comprises the following steps:
the effervescent tablets and water are mixed according to the dosage ratio of 60g to 1L to form the hydromagnetic suspension, then the hydromagnetic suspension is sprayed on the surface of a 20# steel workpiece, the workpiece surface is magnetized by a magnetic probe machine and the defects on the workpiece surface are detected, the cracks with the width of 0.1 mu m and the length of 0.5 mu m can be detected, and the detection sensitivity is high.

Claims (10)

1. An effervescent tablet containing nano magnetic powder is characterized by comprising the following components: nano magnetic powder, a dispersing agent, a defoaming agent, a forming agent, alkaline carbonate and a film-forming agent; the nanometer magnetic powder is nanometer Fe2O3
2. Effervescent tablet according to claim 1, wherein the nano-Fe is2O3Is nano gamma-Fe2O3
3. The effervescent tablet of claim 1, wherein the nanomagnetic powder has a particle size of 1-100 nm.
4. The effervescent tablet of claim 1, wherein the dispersing agent is selected from at least one of polyoxyethylene polyoxypropylene block copolymer, triethanolamine, or sodium benzoate.
5. The effervescent tablet of claim 1, further comprising a sulfate and/or trichloroisocyanuric acid.
6. The effervescent tablet of claim 1, comprising the following components in percentage by mass: 20-35% of nano magnetic powder, 30-40% of dispersing agent, 1-3% of defoaming agent, 5-15% of forming agent, 3-7% of alkaline carbonate and the balance of film-forming agent.
7. The effervescent tablet of claim 5, comprising the following components in percentage by mass: 25% of nano magnetic powder, 13% of polyoxyethylene polyoxypropylene block copolymer, 7% of triethanolamine, 12% of sodium benzoate, 3% of defoaming agent, 10% of forming agent, 5% of alkaline carbonate, 2% of film-forming agent, 15% of magnesium sulfate and 8% of trichloroisocyanuric acid.
8. A process for the preparation of an effervescent tablet as claimed in any one of claims 1 to 7, comprising the steps of:
weighing the components according to the formula ratio, mixing the nano magnetic powder with the film forming agent, then adding the other components except the forming agent, stirring and mixing, then adding the forming agent, stirring and mixing, tabletting and forming to obtain the effervescent tablet.
9. The preparation method according to claim 8, wherein the film forming agent is mixed with water to prepare a solution with a mass concentration of 8-12%, and then mixed with the nano magnetic powder.
10. A method of using the effervescent tablet of any one of claims 1-7, comprising the steps of:
and mixing the effervescent tablets with water to form a water magnetic suspension, spraying the water magnetic suspension on the surface of a workpiece, magnetizing the workpiece by using a magnetic detector and detecting the defect data of the workpiece.
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