CN110355353A - A kind of preparation method of cracking resistance gap type metal infiltration agent material - Google Patents
A kind of preparation method of cracking resistance gap type metal infiltration agent material Download PDFInfo
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- CN110355353A CN110355353A CN201910505639.8A CN201910505639A CN110355353A CN 110355353 A CN110355353 A CN 110355353A CN 201910505639 A CN201910505639 A CN 201910505639A CN 110355353 A CN110355353 A CN 110355353A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D31/00—Cutting-off surplus material, e.g. gates; Cleaning and working on castings
- B22D31/002—Cleaning, working on castings
- B22D31/005—Sealing or impregnating porous castings
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F3/26—Impregnating
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Abstract
The present invention relates to a kind of cracking resistance gap type metal preparation methods of infiltration agent material, belong to metal processing auxiliary agent technical field.Technical solution of the present invention uses water soluble peroxygen metatitanic acid for raw material, pass through the transparent Anatase colloidal sol of hydro-thermal method low temperature preparation, for modified matrix, it will be permeated in low concentration colloidal sol, the macropore being filled in metal material inside, it mentions so that internal form more effectively filling and combine, simultaneously, the sol-fraction of interior infiltration can contact the region surface formed in contact by poriferous titanium dioxide particulate interspaces with material matrix, form fine and close barrier layer, technical solution of the present invention using sulfonation modifying salicylic acid and is adsorbed in gel rubber material simultaneously, due to salicylic acid structure, the composite material of stronger coordination ability is formed with metal porous material surface, promote metal pore interior, being cross-linked with each other between colloidal sol packing material and cured modified material three, increase bond strength, reduce material cracks performance.
Description
Technical field
The present invention relates to a kind of cracking resistance gap type metal preparation methods of infiltration agent material, belong to metal processing auxiliary agent technology
Field.
Background technique
It casts components and powder sintered components in process of production, micropore or gap, such as needle inevitably occurs
The product defects such as hole, stomata, loose, for ratio of defects according to the shape of product, thickness, size and difference, ratio of defects is 6~100%.
For there is the product of air-tightness requirement, after machining, discovery leakage can only then scrap when pressure test, to cause people
The waste of work, raw material, the energy etc..The product of no air-tightness requirement is when plating, spraying, plastic-spraying etc. are surface-treated, because of cleaning
The media such as agent, acid solution enter hole, lead to internal corrosion, shorten the working life, or because the presence of micropore makes process of surface treatment
There is bubble or uneven phenomenon, leads to product quality defect.To handle problems, need to infiltrate processing, in certain item
Impregnant is penetrated into the micropore of casting under part, and polymerize impregnant in hole by heating and forms colloid, thus
It is filled with the hole of components.
Mainly there are silicic acid sodium form impregnant, the agent of acrylic ester type organic impregnating and resin type using extensive impregnant at present
Impregnant three categories.Inorganic impregnant is a kind of impregnant used earliest, there is that low in cost, heat resistance is strong, but
Its viscosity is high, wellability is poor, infiltration qualification rate is low, just gradually replaced acrylic ester type impregnant.Resin type impregnant
Due to viscosity is excessive, needs to be added diluent and be diluted, in diluent many be more toxic it is higher with volatility
Compound, detrimental effect is all brought to environmental protection and safety, infiltration yield rate, thus just gradually by acrylic ester type impregnant
It is replaced.Acrylic ester type impregnant is not because have the shortcomings that silicic acid sodium form and resin type impregnant, gradually instead of other classes
The impregnant of type is a kind of impregnant for most having application prospect now, and acrylic ester type impregnant forms substantially mainly includes
Functional form acrylate monomer, acrylate oligomer, initiator, polymerization inhibitor, anti-shrink ingredient, emulsifier, chelating agent etc..Third
Olefin(e) acid ester type impregnant advantage is not shunk after acrylic ester type impregnant solidifies in hole, it is possible to fully plugging hole
Gap infiltrates success rate highest, the another tolerance under the various physical and chemical conditions such as irreversible, heat-resisting, solvent resistant after solidifying.
The critical material of impregnation technology is organic impregnating agent, and this kind of material main component is low viscosity heat cure (methyl) third
Olefin(e) acid ester monomer mixture, has a disadvantage in that: (methyl) acrylate monomer cure shrinkage is big, and the shrinking percentage of many monomers exists
15%, cause impregnant to be easy to appear slight crack and secondary contraction gap in the curing process, influences repairing effect, especially repair
Casting gap it is larger when.
In addition the organic impregnating agent washing property being commercialized at present is not so good, and after the completion of infiltration, when cast(ing) surface often goes out
It is existing some because of there is no wash clean to lead to cured white residue glue solidfied material, influence cast(ing) surface appearance and assembly.Summary of the invention
The technical problems to be solved by the invention: cause impregnant solid greatly for (methyl) acrylate monomer cure shrinkage
The problem of being easy to appear slight crack and secondary contraction gap during changing, influence repairing effect, provides a kind of cracking resistance gap type metal
With the preparation method of infiltration agent material.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
(1) according to parts by weight, 45~50 parts of epoxy resin, 3~5 parts of polymerization inhibitors, 1~2 part of palladium catalyst is weighed respectively to be placed in
In three-necked flask, it is stirred juxtaposition at room temperature, 88~92 DEG C is warming up to by 2 DEG C/min, after 1~2h of insulation reaction, to three
Methacrylic acid is added dropwise in mouthful flask, after being added dropwise to complete, 2~3h of insulation reaction, then to epoxy resin is added dropwise in three-necked flask
The toluene di-isocyanate(TDI) of quality 10%, 2~3h of insulation reaction, is prepared into compound osmsticum；
(2) 5% ammonium hydroxide of mass fraction is added dropwise in 15% titanium sulfate solution of mass fraction, is stirred by 1:10 in mass ratio
And insulation reaction, it collects reaction solution and standing is cooled to room temperature, be centrifugated, collect lower sediment and 1:10 in mass ratio, it will
Lower sediment is stirred and stands with hydrogenperoxide steam generator, collects sol solutions, 1:10, sol solutions are added to by volume
In ionized water, hydro-thermal reaction, standing is cooled to room temperature, and obtains sol matrix liquid；
(3) salicylic acid and 1:5 in mass ratio are taken, salicylic acid is added in deionized water, is stirred and is added dropwise sulfuric acid, is stirred
It mixes and keeps the temperature sulfonation processing, standing is cooled to room temperature, collects to obtain modification liquid, modification liquid is added in sol matrix liquid, is stirred
Mixing and ultrasonic disperse are mixed, dispersion liquid is collected to obtain；
(4) dispersion liquid, compound osmsticum, acrylic monomers, para hydroxybenzene phenol, azodiisobutyronitrile and ethylene glycol is weighed respectively to set
In beaker, the cracking resistance gap type metal infiltration agent material can be prepared by being stirred.
Polymerization inhibitor described in step (1) is preferably p-tert-Butylcatechol polymerization inhibitor.
Epoxy resin described in step (1) is preferably epoxy resin E-41.
Methacrylic acid dripping quantity described in step (1) is epoxy resin quality 1/2.
Time for adding described in step (1) is 3~4h.
5% ammonium hydroxide drop rate of mass fraction described in step (2) is 2~3mL/min.
Hydrothermal temperature described in step (3) is 100~120 DEG C.
Mixed proportion is 1:5 by volume between modification liquid and sol matrix liquid described in step (3).
Dropwise addition sulfuric acid described in step (3) is that control drop rate is 1~2mL/min, and quality and deionized water is added dropwise
It measures identical.
It is mixed between dispersion liquid described in step (4), acrylic monomers, para hydroxybenzene phenol, azodiisobutyronitrile and ethylene glycol
Composition and division in a proportion example is according to parts by weight, to weigh 45~50 parts of dispersion liquids, 10~15 parts of compound osmsticums, 10~15 parts of acrylic acid respectively
Monomer, 3~5 parts of para hydroxybenzene phenol, 1~2 part of azodiisobutyronitrile and 15~20 parts of ethylene glycol.
The present invention is compared with other methods, and advantageous effects are:
(1) technical solution of the present invention uses water soluble peroxygen metatitanic acid for raw material, passes through the transparent Anatase of hydro-thermal method low temperature preparation
Colloidal sol is modified matrix, will permeate in low concentration colloidal sol, the macropore being filled in metal material inside improves metal hole
Internal bridged effect between particle, so that internal form more effectively filling and combine, meanwhile, the sol-fraction meeting of interior infiltration
The region surface formed in contact is contacted with material matrix by poriferous titanium dioxide particulate interspaces, forms fine and close barrier layer,
Technical solution of the present invention using sulfonation modifying salicylic acid and is adsorbed in gel rubber material simultaneously, due to salicylic acid structure, with metal
Porous material surface forms the composite material of stronger coordination ability, promotes metal pore interior, colloidal sol packing material and consolidates
Change being cross-linked with each other between modified material three, hence it is evident that increase bond strength, material cracks performance is effectively reduced；
(2) technical solution of the present invention uses epoxide synthesizing new methacrylic acid based isocyanate, by making it effectively
It infiltrates into inside metal material, in the case where being contacted with oxygen (air), due to the inhibition of oxygen, esters of acrylic acid list
Polymerization reaction does not occur for body, and at starvation (air), then start rapidly to polymerize and solidify, to play bonding, sealing
Effect, so, technical solution of the present invention uses with unique self-curing and adjusts the ability of curing rate, becomes sealing
The most reliable sealing material of metal and non-metallic component hole, the sealant of liquid have the tendency that nature polymerization, but by packet
This polymerization can be prevented by penetrating into a small amount of air in dress object and keeping constant the method for temperature, while being had to micropore and actively being infiltrated
Property, when modified penetrating fluid enters part hole, it no longer has stable air source, and starts chemosetting, with gold
Belonging to contacted with ions can promote solidification, this is similar to certain chemical catalysts, however heating, catalyst and metal ion are to solidification process
It is not necessary condition, but the speed of their adjustable curing reactions, and by controlling curing reaction speed in each infiltration process
Degree is not in spillover to obtain best infiltration effect, therefore component will not be besmirched, and sealing performance is stablized, self-curing
Reliability, it can be ensured that the components infiltrated are non-leakage.
Specific embodiment
According to parts by weight, 45~50 parts of epoxy resin, 3~5 parts of polymerization inhibitor p-tert-Butylcatechols, 1 are weighed respectively
~2 parts of palladium catalysts are placed in three-necked flask, are stirred juxtaposition at room temperature, are warming up to 88~92 DEG C by 2 DEG C/min, heat preservation
After reacting 1~2h, to the methacrylic acid that epoxy resin quality 1/2 is added dropwise in three-necked flask, control time for adding is 3~4h,
After being added dropwise to complete, 2~3h of insulation reaction, then in three-necked flask be added dropwise epoxy resin quality 10% toluene di-isocyanate(TDI),
2~3h of insulation reaction, is prepared into compound osmsticum；5% ammonium hydroxide of mass fraction is added dropwise to mass fraction by 1:10 in mass ratio
In 15% titanium sulfate solution, control drop rate be 2~3mL/min, be stirred be placed in insulation reaction 1 at 70~80 DEG C~
2h, collects reaction solution and standing is cooled to room temperature, then is centrifugated at 1500~2000r/min, collects lower sediment and simultaneously presses
Lower sediment and 25% hydrogenperoxide steam generator of mass fraction are stirred and are stood 6~8h, collect sol solutions by mass ratio 1:10
And 1:10 by volume, sol solutions are added in deionized water, the hydro-thermal reaction 20~for 24 hours at 100~120 DEG C is stood cold
But to room temperature, sol matrix liquid is obtained；Salicylic acid and in mass ratio 1:5 are taken, salicylic acid is added in deionized water, is stirred
And 80% sulfuric acid of mass fraction is added dropwise, control drop rate is 1~2mL/min, and dropwise addition quality is identical as deionized water quality, is stirred
It mixes mixing and is placed at 75~80 DEG C and keep the temperature sulfonation and handle 1~2h, standing is cooled to room temperature, and collects to obtain modification liquid and by volume
Modification liquid is added in sol matrix liquid by 1:5, is stirred and is placed in 10~15min of ultrasonic disperse under 200~300W, is received
Collect to obtain dispersion liquid；According to parts by weight, 45~50 parts of dispersion liquids, 10~15 parts of compound osmsticums, 10~15 part third are weighed respectively
Acrylic monomer, 3~5 parts of para hydroxybenzene phenol, 1~2 part of azodiisobutyronitrile and 15~20 parts of ethylene glycol are placed in a beaker, and stirring is mixed
The cracking resistance gap type metal infiltration agent material can be prepared by closing.
Example 1
According to parts by weight, 45 parts of epoxy resin, 3 parts of polymerization inhibitor p-tert-Butylcatechols, 1 part of palladium catalyst is weighed respectively to set
In three-necked flask, it is stirred juxtaposition at room temperature, 88 DEG C is warming up to by 2 DEG C/min, after insulation reaction 1h, to three-necked flask
The middle methacrylic acid that epoxy resin quality 1/2 is added dropwise, control time for adding is 3h, after being added dropwise to complete, insulation reaction 2h, then
To the toluene di-isocyanate(TDI) that epoxy resin quality 10% is added dropwise in three-necked flask, insulation reaction 2h is prepared into compound osmsticum；
5% ammonium hydroxide of mass fraction is added dropwise in 15% titanium sulfate solution of mass fraction by 1:10 in mass ratio, and control drop rate is
2mL/min is stirred and is placed in insulation reaction 1h at 70 DEG C, collects reaction solution and standing is cooled to room temperature, then in 1500r/
It is centrifugated under min, lower sediment and 1:10 in mass ratio is collected, by lower sediment and 25% hydrogenperoxide steam generator of mass fraction
It is stirred and is stood 6h, sol solutions and by volume 1:10 is collected, sol solutions is added in deionized water, at 100 DEG C
Hydro-thermal reaction 20h, standing are cooled to room temperature, and obtain sol matrix liquid；Salicylic acid and in mass ratio 1:5 are taken, salicylic acid is added to
In deionized water, it is stirred and is added dropwise 80% sulfuric acid of mass fraction, control drop rate is 1mL/min, and quality is added dropwise and goes
Ionized water is identical in quality, is stirred to be placed at 75 DEG C and keeps the temperature sulfonation processing 1h, and standing is cooled to room temperature, and collects to obtain modification liquid
And 1:5 by volume, modification liquid is added in sol matrix liquid, is stirred and is placed in ultrasonic disperse 10min under 200W, is received
Collect to obtain dispersion liquid；According to parts by weight, 45 parts of dispersion liquids, 10 parts of compound osmsticums, 10 parts of acrylic monomers, 3 parts are weighed respectively
Para hydroxybenzene phenol, 1 part of azodiisobutyronitrile and 15 parts of ethylene glycol are placed in a beaker, and the cracking resistance can be prepared by being stirred
Gap type metal infiltration agent material.
Example 2
According to parts by weight, 46 parts of epoxy resin, 4 parts of polymerization inhibitor p-tert-Butylcatechols, 1.3 parts of palladium catalysts are weighed respectively
It is placed in three-necked flask, is stirred juxtaposition at room temperature, 89 DEG C are warming up to by 2 DEG C/min, after insulation reaction 1.3h, to three mouthfuls
The methacrylic acid of epoxy resin quality 1/2 is added dropwise in flask, control time for adding is 3.3h, and after being added dropwise to complete, heat preservation is anti-
2.3h is answered, then to the toluene di-isocyanate(TDI) that epoxy resin quality 10% is added dropwise in three-necked flask, insulation reaction 2.3h is prepared into
Compound osmsticum；5% ammonium hydroxide of mass fraction is added dropwise in 15% titanium sulfate solution of mass fraction by 1:10 in mass ratio, control
Drop rate is 2.3mL/min, is stirred and is placed in insulation reaction 1.3h at 73 DEG C, collects reaction solution and standing is cooled to room
Temperature, then be centrifugated at 1670r/min, lower sediment and 1:10 in mass ratio are collected, by lower sediment and mass fraction
25% hydrogenperoxide steam generator is stirred and stands 6.7h, collects sol solutions and by volume 1:10, sol solutions are added to
In ionized water, hydro-thermal reaction 21h, standing are cooled to room temperature at 107 DEG C, obtain sol matrix liquid；Take salicylic acid and in mass ratio
Salicylic acid is added in deionized water by 1:5, is stirred and is added dropwise 80% sulfuric acid of mass fraction, and control drop rate is
1.3mL/min, dropwise addition quality is identical as deionized water quality, is stirred and is placed in heat preservation sulfonation processing 1.3h at 76 DEG C, quiet
It sets and is cooled to room temperature, collect to obtain modification liquid and 1:5 by volume, modification liquid is added in sol matrix liquid, is stirred simultaneously
It is placed in ultrasonic disperse 12min under 230W, collects to obtain dispersion liquid；According to parts by weight, respectively weigh 46 parts of dispersion liquids, 11 parts it is compound
Penetrating fluid, 12 parts of acrylic monomers, 3.7 parts of para hydroxybenzene phenol, 1.3 parts of azodiisobutyronitriles and 16 parts of ethylene glycol are placed in beaker
In, the cracking resistance gap type metal infiltration agent material can be prepared by being stirred.
Example 3
According to parts by weight, 48 parts of epoxy resin, 4 parts of polymerization inhibitor p-tert-Butylcatechols, 2 parts of palladium catalysts are weighed respectively to set
In three-necked flask, it is stirred juxtaposition at room temperature, is warming up to 91 DEG C by 2 DEG C/min, after insulation reaction 1.5h, three mouthfuls are burnt
The methacrylic acid of epoxy resin quality 1/2 is added dropwise in bottle, control time for adding is 3.5h, after being added dropwise to complete, insulation reaction
2.5h, then to the toluene di-isocyanate(TDI) that epoxy resin quality 10% is added dropwise in three-necked flask, insulation reaction 2.5h is prepared into multiple
Close penetrating fluid；5% ammonium hydroxide of mass fraction is added dropwise in 15% titanium sulfate solution of mass fraction by 1:10 in mass ratio, control drop
Rate of acceleration is 2.6mL/min, is stirred and is placed in insulation reaction 1.5h at 76 DEG C, collects reaction solution and standing is cooled to room
Temperature, then be centrifugated at 1750r/min, lower sediment and 1:10 in mass ratio are collected, by lower sediment and mass fraction
25% hydrogenperoxide steam generator is stirred and stands 7.5h, collects sol solutions and by volume 1:10, sol solutions are added to
In ionized water, hydro-thermal reaction 23h, standing are cooled to room temperature at 115 DEG C, obtain sol matrix liquid；Take salicylic acid and in mass ratio
Salicylic acid is added in deionized water by 1:5, is stirred and is added dropwise 80% sulfuric acid of mass fraction, and control drop rate is
1.6.mL/min, it is identical as deionized water quality that quality is added dropwise, is stirred and is placed in heat preservation sulfonation processing 1.6h at 78 DEG C, it is quiet
It sets and is cooled to room temperature, collect to obtain modification liquid and 1:5 by volume, modification liquid is added in sol matrix liquid, is stirred simultaneously
It is placed in ultrasonic disperse 14min under 265W, collects to obtain dispersion liquid；According to parts by weight, respectively weigh 48 parts of dispersion liquids, 14 parts it is compound
Penetrating fluid, 14 parts of acrylic monomers, 4 parts of para hydroxybenzene phenol, 2 parts of azodiisobutyronitriles and 18 parts of ethylene glycol are placed in a beaker, and are stirred
The cracking resistance gap type metal infiltration agent material can be prepared by mixing mixing.
Example 4
According to parts by weight, 50 parts of epoxy resin, 5 parts of polymerization inhibitor p-tert-Butylcatechols, 2 parts of palladium catalysts are weighed respectively to set
In three-necked flask, it is stirred juxtaposition at room temperature, 92 DEG C is warming up to by 2 DEG C/min, after insulation reaction 2h, to three-necked flask
The middle methacrylic acid that epoxy resin quality 1/2 is added dropwise, control time for adding is 4h, after being added dropwise to complete, insulation reaction 3h, then
To the toluene di-isocyanate(TDI) that epoxy resin quality 10% is added dropwise in three-necked flask, insulation reaction 3h is prepared into compound osmsticum；
5% ammonium hydroxide of mass fraction is added dropwise in 15% titanium sulfate solution of mass fraction by 1:10 in mass ratio, and control drop rate is
3mL/min is stirred and is placed in insulation reaction 2h at 80 DEG C, collects reaction solution and standing is cooled to room temperature, then in 2000r/
It is centrifugated under min, lower sediment and 1:10 in mass ratio is collected, by lower sediment and 25% hydrogenperoxide steam generator of mass fraction
It is stirred and is stood 8h, sol solutions and by volume 1:10 is collected, sol solutions is added in deionized water, at 120 DEG C
For 24 hours, standing is cooled to room temperature hydro-thermal reaction, obtains sol matrix liquid；Salicylic acid and in mass ratio 1:5 are taken, salicylic acid is added to
In deionized water, it is stirred and is added dropwise 80% sulfuric acid of mass fraction, control drop rate is 2mL/min, and quality is added dropwise and goes
Ionized water is identical in quality, is stirred to be placed at 80 DEG C and keeps the temperature sulfonation processing 2h, and standing is cooled to room temperature, and collects to obtain modification liquid
And 1:5 by volume, modification liquid is added in sol matrix liquid, is stirred and is placed in ultrasonic disperse 15min under 300W, is received
Collect to obtain dispersion liquid；According to parts by weight, 50 parts of dispersion liquids, 15 parts of compound osmsticums, 15 parts of acrylic monomers, 5 parts are weighed respectively
Para hydroxybenzene phenol, 2 parts of azodiisobutyronitriles and 20 parts of ethylene glycol are placed in a beaker, and the cracking resistance can be prepared by being stirred
Gap type metal infiltration agent material.
Cracking resistance gap type metal prepared by the present invention is examined with infiltration agent material and commercially available metal with infiltration agent material
It surveys, specific testing result such as following table table 1:
Test method:
Stability: being placed on 75 DEG C of oil baths for impregnant loading test tube, and the time of gel occurs in measurement, if gel time >=
20min indicates qualified, otherwise unqualified；
Curing rate: impregnant loading test tube is placed on 90 DEG C of oil baths, the time of gel just occurs in test；
Cubical contraction: hydrometer method and drainage measurement is respectively adopted
Glue density (ρ a) and cured glue stick density (ρ c) before organic impregnating sealant cures, then shrinking percentage=(ρ c- ρ a)/ρ
c；
Washing property: upper and lower, the left each M8 threaded hole for vertically making a call to a depth 20mm in three faces by 30mm × 30mm × 30mm aluminium block,
Taking-up after this test specimen is immersed in impregnant swings cleaning 5min in originally sink, is subsequently placed in 90 DEG C of hot water storgaes solid
It is taken out after changing 15min, whether observe in surface of test piece and all threaded holes has residue glue.
1 cracking resistance gap type metal of table is characterized with impregnant material property
Cracking resistance gap type metal prepared by the present invention infiltration agent material as shown in Table 1, stability is good, and cubical contraction is low, washing
Good, the noresidue of property, has a vast market value and application prospect.
Claims (10)
1. a kind of cracking resistance gap type metal preparation method of infiltration agent material, it is characterised in that have preparation step are as follows:
(1) according to parts by weight, 45~50 parts of epoxy resin, 3~5 parts of polymerization inhibitors, 1~2 part of palladium catalyst is weighed respectively to be placed in
In three-necked flask, it is stirred juxtaposition at room temperature, 88~92 DEG C is warming up to by 2 DEG C/min, after 1~2h of insulation reaction, to three
Methacrylic acid is added dropwise in mouthful flask, after being added dropwise to complete, 2~3h of insulation reaction, then to epoxy resin is added dropwise in three-necked flask
The toluene di-isocyanate(TDI) of quality 10%, 2~3h of insulation reaction, is prepared into compound osmsticum；
(2) 5% ammonium hydroxide of mass fraction is added dropwise in 15% titanium sulfate solution of mass fraction, is stirred by 1:10 in mass ratio
And insulation reaction, it collects reaction solution and standing is cooled to room temperature, be centrifugated, collect lower sediment and 1:10 in mass ratio, it will
Lower sediment is stirred and stands with hydrogenperoxide steam generator, collects sol solutions, 1:10, sol solutions are added to by volume
In ionized water, hydro-thermal reaction, standing is cooled to room temperature, and obtains sol matrix liquid；
(3) salicylic acid and 1:5 in mass ratio are taken, salicylic acid is added in deionized water, is stirred and is added dropwise sulfuric acid, is stirred
It mixes and keeps the temperature sulfonation processing, standing is cooled to room temperature, collects to obtain modification liquid, modification liquid is added in sol matrix liquid, is stirred
Mixing and ultrasonic disperse are mixed, dispersion liquid is collected to obtain；
(4) dispersion liquid, compound osmsticum, acrylic monomers, para hydroxybenzene phenol, azodiisobutyronitrile and ethylene glycol is weighed respectively to set
In beaker, the cracking resistance gap type metal infiltration agent material can be prepared by being stirred.
2. a kind of preparation method of cracking resistance gap type metal infiltration agent material according to claim 1, it is characterised in that: step
Suddenly polymerization inhibitor described in (1) is preferably p-tert-Butylcatechol polymerization inhibitor.
3. a kind of preparation method of cracking resistance gap type metal infiltration agent material according to claim 1, it is characterised in that: step
Suddenly epoxy resin described in (1) is preferably epoxy resin E-41.
4. a kind of preparation method of cracking resistance gap type metal infiltration agent material according to claim 1, it is characterised in that: step
Suddenly methacrylic acid dripping quantity described in (1) is epoxy resin quality 1/2.
5. a kind of preparation method of cracking resistance gap type metal infiltration agent material according to claim 1, it is characterised in that: step
Suddenly time for adding described in (1) is 3~4h.
6. a kind of preparation method of cracking resistance gap type metal infiltration agent material according to claim 1, it is characterised in that: step
Suddenly 5% ammonium hydroxide drop rate of mass fraction described in (2) is 2~3mL/min.
7. a kind of preparation method of cracking resistance gap type metal infiltration agent material according to claim 1, it is characterised in that: step
Suddenly hydrothermal temperature described in (3) is 100~120 DEG C.
8. a kind of preparation method of cracking resistance gap type metal infiltration agent material according to claim 1, it is characterised in that: step
Suddenly mixed proportion is 1:5 by volume between modification liquid and sol matrix liquid described in (3).
9. a kind of preparation method of cracking resistance gap type metal infiltration agent material according to claim 1, it is characterised in that: step
Suddenly it is 1~2mL/min that dropwise addition sulfuric acid described in (3), which is control drop rate, and it is identical as deionized water quality that quality is added dropwise.
10. a kind of preparation method of cracking resistance gap type metal infiltration agent material according to claim 1, it is characterised in that:
Mixed proportion is between dispersion liquid described in step (4), acrylic monomers, para hydroxybenzene phenol, azodiisobutyronitrile and ethylene glycol
According to parts by weight, respectively weigh 45~50 parts of dispersion liquids, 10~15 parts of compound osmsticums, 10~15 parts of acrylic monomers, 3~
5 parts of para hydroxybenzene phenol, 1~2 part of azodiisobutyronitrile and 15~20 parts of ethylene glycol.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111590059A (en) * | 2020-05-28 | 2020-08-28 | 安徽凯斯威精工科技有限公司 | Infiltration liquid for copper-nickel/iron-nickel alloy and use method and application thereof |
| CN113913136A (en) * | 2021-10-22 | 2022-01-11 | 南京艾布纳密封技术股份有限公司 | Recycling and reusing type anaerobic osmosis sealant composition and preparation method thereof |
| CN115006607A (en) * | 2022-07-04 | 2022-09-06 | 诺一迈尔(山东)医学科技有限公司 | Repairing film and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60120780A (en) * | 1983-12-02 | 1985-06-28 | Mitsubishi Rayon Co Ltd | Method for impregnating porous article and sealing pore |
| CN105061670A (en) * | 2015-08-06 | 2015-11-18 | 南京艾布纳密封技术有限公司 | Low-contraction acrylic acid ester vacuum infiltration agent used for sealed reinforcement |
| CN105921725A (en) * | 2016-05-30 | 2016-09-07 | 初丽萍 | Method for magnetic nanoparticle modified methacrylate magnetic impregnant for metal castings |
| CN106632902A (en) * | 2016-12-14 | 2017-05-10 | 湖北回天新材料股份有限公司 | Low-shrinkage heat-cured organic infiltration agent and preparation method thereof |
| CN106957386A (en) * | 2017-05-02 | 2017-07-18 | 南京艾布纳密封技术股份有限公司 | A kind of water-resistant type impregnant |
| CN106995514A (en) * | 2017-05-02 | 2017-08-01 | 南京艾布纳密封技术股份有限公司 | A kind of high metal attached type methacrylate organic impregnating agent |
-
2019
- 2019-06-12 CN CN201910505639.8A patent/CN110355353A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60120780A (en) * | 1983-12-02 | 1985-06-28 | Mitsubishi Rayon Co Ltd | Method for impregnating porous article and sealing pore |
| CN105061670A (en) * | 2015-08-06 | 2015-11-18 | 南京艾布纳密封技术有限公司 | Low-contraction acrylic acid ester vacuum infiltration agent used for sealed reinforcement |
| CN105921725A (en) * | 2016-05-30 | 2016-09-07 | 初丽萍 | Method for magnetic nanoparticle modified methacrylate magnetic impregnant for metal castings |
| CN107538000A (en) * | 2016-05-30 | 2018-01-05 | 初丽萍 | The method of metal casting magnetic modified nanometer methacrylate magnetic impregnant |
| CN106632902A (en) * | 2016-12-14 | 2017-05-10 | 湖北回天新材料股份有限公司 | Low-shrinkage heat-cured organic infiltration agent and preparation method thereof |
| CN106957386A (en) * | 2017-05-02 | 2017-07-18 | 南京艾布纳密封技术股份有限公司 | A kind of water-resistant type impregnant |
| CN106995514A (en) * | 2017-05-02 | 2017-08-01 | 南京艾布纳密封技术股份有限公司 | A kind of high metal attached type methacrylate organic impregnating agent |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111590059A (en) * | 2020-05-28 | 2020-08-28 | 安徽凯斯威精工科技有限公司 | Infiltration liquid for copper-nickel/iron-nickel alloy and use method and application thereof |
| CN113913136A (en) * | 2021-10-22 | 2022-01-11 | 南京艾布纳密封技术股份有限公司 | Recycling and reusing type anaerobic osmosis sealant composition and preparation method thereof |
| CN115006607A (en) * | 2022-07-04 | 2022-09-06 | 诺一迈尔(山东)医学科技有限公司 | Repairing film and preparation method thereof |
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