CN104388944B - A kind of microencapsulation vapor phase inhibitor and preparation method thereof - Google Patents
A kind of microencapsulation vapor phase inhibitor and preparation method thereof Download PDFInfo
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- CN104388944B CN104388944B CN201410728957.8A CN201410728957A CN104388944B CN 104388944 B CN104388944 B CN 104388944B CN 201410728957 A CN201410728957 A CN 201410728957A CN 104388944 B CN104388944 B CN 104388944B
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- core
- wall material
- vapor phase
- microencapsulation
- phase inhibitor
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Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
- C23F11/02—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in air or gases by adding vapour phase inhibitors
Abstract
The present invention relates to a kind of microencapsulation vapor phase inhibitor, phosphoric acid dihydro zinc, phosphate dihydrogen manganese, nickel nitrate, sodium fluoride, sodium nitrate, phosphoric acid, citric acid, phosphotungstic acid, sodium molybdate.In the present invention, each component mix with deionized water after finished product.When using; neodymium-iron-boron magnetic material is put into ultrasound wave barrel; adjusted according to oil removing, cleaning, table, neodymium iron boron special surface treating agent is processed, close and the order of drying is processed; first micro- rust on surface is removed; and form the diaphragm of even compact on surface; neodymium-iron-boron magnetic material is weightless few after treatment, and salt water immersion test shows more resistant to corrosion, and reduces harm of the strong acid pickling to environment and operating personnel.
Description
Technical field
The invention belongs to metallic article technical field of rust prevention, especially a kind of microencapsulation vapor phase inhibitor and its preparation side
Method.
Background technology
Metallic article can be subject to what is got rusty to endanger during shipping storage, and its main cause is relative humidity of atomsphere, gas
Temperature and humidity, corrosive gas and other corrosion factors, people plate compared with frequently with top layer brushing Erosion-Resisting Non-metallic Materials, top layer
Upper corrosion resistant metal, chemical method form the methods such as sull, and with the development of science and technology, vapor phase inhibitor technology is more next
It is more welcomed by the people, its be by special synthesis technique, a kind of corrosion inhibitor for being prepared from of compounding, can individually or according to
Suitable carrier is invested, at normal temperatures and pressures direct gasification, can be full of in any spatial gaps in sealed environment, and absorption exists
Metal surface, forms very thin fine and close protection film layer, effective exclusion of water, oxygen and other corrosion factors, and suppression promotes metal rotten
The electrochemical reaction of erosion, so as to reach optimal anti-corrosion effect.
Because the vapour phase inhibitor release sustained-release particle free degree is high, so its rate of release is uncontrollable, thus cause gas phase
The shortcoming that corrosion inhibiter usage cycles are short, usage amount is big, negative effect is brought to national economy and environment.As can be seen here, how
The rate of release of corrosion inhibiter is reduced, it is an important problem using total amount to extend corrosion inhibiter usage cycles, control it, is not only saved
About use cost and be conducive to preserving the ecological environment.
The content of the invention
It is an object of the invention to overcome the deficiencies in the prior art, there is provided the one of scientific matching, sustained release and favorable rust preventing effect
Plant microencapsulation vapor phase inhibitor.
The present invention is adopted the technical scheme that:
A kind of microencapsulation vapor phase inhibitor, it is characterised in that:Including core and wall material, wall material is wrapped in outside core and is formed
Microcapsules, the core includes octadecane butyl diacid, 1, the alkenyl imidazoline of 2- aminoethyls 17, lanolin, BTA
And base oil, the wall material is synthesis macromolecular material.
And, also including curing agent and emulsifying agent.
And, the core includes the following components for mixing by weight percentage:
The core is 1 with the weight ratio of wall material:2~5.
And, the wall material is by the cyanurotriamide modified polymer for obtaining urea and formaldehyde.
And, the wall material is the polymer of melamine and formaldehyde.
And, the wall material is polyvinyl alcohol.
It is a further object to provide a kind of preparation method of microencapsulation vapor phase inhibitor, it is characterised in that:
Comprise the following steps:
(1) formaldehyde is mixed with urea, heated, pH adjusting agent is then added dropwise pH is adjusted to 8, insulation reaction;
(2) sticky performed polymer is obtained after continuously adding melamine reaction;
(3) NP-10 in core addition deionized water, will be added, insulated and stirred forms uniform tiny dispersed oil droplets;
(4) during the product by step (2) adds step product (3), acetic acid is added dropwise, it is 2.5 to adjust pH after stirring, after reaction
To micro-capsule dispersion liquid;
(5) the product after suction filtration is washed with formaldehyde, finished product after drying.
It is a further object to provide a kind of preparation method of microencapsulation vapor phase inhibitor, it is characterised in that:
Comprise the following steps:
(1) formaldehyde and water are added in melamine, pH adjusting agent is subsequently adding and pH is adjusted to 8~9, after heating response
To the performed polymer aqueous solution of carbamide;
(2) NP-10 and core are mixed, add pH adjusting agent and pH is adjusted to 4.5, it is fully emulsified under strong agitation;
(3) step product (1), insulated and stirred are added in step product (2), then pH is adjusted to 9 with pH adjusting agent, obtained
To micro-capsule dispersion liquid;
(4) washed with formaldehyde after suction filtration, finished product after drying.
It is a further object to provide a kind of preparation method of microencapsulation vapor phase inhibitor, it is characterised in that:
Comprise the following steps:
(1) added after polyvinyl alcohol is mixed with OP-10 in deionized water, add pH adjusting agent that pH is adjusted to 10, obtain water
Phase;
(2) core is mixed to be dissolved in carbon tetrachloride solution and obtain organic phase;
(3) strong agitation is fully emulsified after the product by step (1) with step (2) mixes, and ethylenediamine is added dropwise, and is obtained after reaction
The microcapsules of solidification.
And, the particle diameter after the wall material parcel core is 3~100 microns.
Advantages and positive effects of the present invention are:
In the present invention, the gas-phase slow-release agent of core using octadecane butyl diacid, 1, the alkenyl imidazoline of 2- aminoethyls 17,
The composition of lanolin, BTA and base oil, wall material can be cyanurotriamide modified urea and formaldehyde polymer,
The polymer or polyvinyl alcohol of melamine and formaldehyde, form footpath and are evenly distributed and intensity preferably micro- glue after wall material parcel core
Capsule.When using by microcapsules taken in one's arms with gauze come, be then placed within sealing chest in, microcapsules slowly discharge gas phase delay
Agent is released, each gap in chest can be full of, it is ensured that the metal works safety of storage in it, the speed of release is slow, anti-corrosion
The time of erosion and effect are good, are especially suitable for the anticorrosion of the metal works of long-term transport or long-term storage.The microcapsules of gained
Particle diameter distribution is uniform, and intensity is preferable.
Brief description of the drawings
Fig. 1 is that embodiment 1 compares figure with unencapsulated gas-phase slow-release agent corrosion inhibition;
Fig. 2 is that embodiment 2 compares figure with unencapsulated gas-phase slow-release agent corrosion inhibition;
Fig. 3 is that embodiment 3 compares figure with unencapsulated gas-phase slow-release agent corrosion inhibition;
Fig. 4 is the stereoscan photograph of microcapsules.
Specific embodiment
With reference to embodiment, the present invention is further described, and following embodiments are illustrative, be not it is limited,
Protection scope of the present invention can not be limited with following embodiments.
A kind of microencapsulation vapor phase inhibitor, innovation of the invention is:Including core and wall material, wall material is wrapped in core
Outer formation microcapsules, the core includes octadecane butyl diacid, 1, the alkenyl imidazoline of 2- aminoethyls 17, lanolin, benzo
Triazole and base oil, the wall material are synthesis macromolecular material.
Also include curing agent and emulsifying agent in said components.Wherein core including mixing with the following group by weight percentage
Point:
Core is 1 with wall material weight ratio therebetween:2~5.
Wall material is macromolecular material, can be following three kinds of components, specifically:1. it is cyanurotriamide modified to obtain urea and formaldehyde
Polymer, the 2. polymer of melamine and formaldehyde, 3. polyvinyl alcohol.
If wall material is 1, the preparation method of microencapsulation vapor phase inhibitor is comprised the following steps:
(1) formaldehyde is mixed with urea, heated, pH adjusting agent is then added dropwise pH is adjusted to 8, insulation reaction;
(2) sticky performed polymer is obtained after continuously adding melamine reaction;
(3) NP-10 in core addition deionized water, will be added, insulated and stirred forms uniform tiny dispersed oil droplets;
(4) during the product by step (2) adds step product (3), acetic acid is added dropwise, it is 2.5 to adjust pH after stirring, after reaction
To micro-capsule dispersion liquid;
(5) the product after suction filtration is washed with formaldehyde, finished product after drying.
If wall material is 2, the preparation method of microencapsulation vapor phase inhibitor, it is characterised in that:Comprise the following steps:
(1) formaldehyde and water are added in melamine, pH adjusting agent is subsequently adding and pH is adjusted to 8~9, after heating response
To the performed polymer aqueous solution of carbamide;
(2) NP-10 and core are mixed, add pH adjusting agent and pH is adjusted to 4.5, it is fully emulsified under strong agitation;
(3) step product (1), insulated and stirred are added in step product (2), then pH is adjusted to 9 with pH adjusting agent, obtained
To micro-capsule dispersion liquid;
(4) washed with formaldehyde after suction filtration, finished product after drying.
If wall material is 3, the preparation method of microencapsulation vapor phase inhibitor, it is characterised in that:Comprise the following steps:
(1) added after polyvinyl alcohol is mixed with OP-10 in deionized water, add pH adjusting agent that pH is adjusted to 10, obtain water
Phase;
(2) core is mixed to be dissolved in carbon tetrachloride solution and obtain organic phase;
(3) strong agitation is fully emulsified after the product by step (1) with step (2) mixes, and ethylenediamine is added dropwise, and is obtained after reaction
The microcapsules of solidification.
No matter which kind of method prepares the microcapsules that wall material wraps up core, the particle diameter of the microcapsules 3~100 microns it
Between.
Embodiment 1
Preparation method is comprised the following steps:
(1) 10.2g formaldehyde is mixed with 24.3g urea, be heated to 70 DEG C, pH adjusting agent triethanolamine is then added dropwise pH
It is adjusted to 8, insulation reaction 1h;
(2) 30g melamines are continuously added, sticky performed polymer is obtained after stirring reaction 1h;
(3) 0.05g NP-10,35 DEG C of stirrings of keeping temperature in 20g cores addition 100ml deionized waters, will be added
30min, forms uniform tiny dispersed oil droplets;
(4) during the product by step (2) adds step product (3), addition speed is 0.5ml/min, and vinegar is added dropwise after stirring 1h
Sour 2.0g, it is 2.5 to adjust pH, and micro-capsule dispersion liquid is obtained after reaction 1h;
(5) the product after suction filtration is washed 3 times with formaldehyde, finished product after 30~40 DEG C of dryings.
Embodiment 2
Preparation method is comprised the following steps:
(1) 15g formaldehyde and 25g water are added in 10g melamines, pH adjusting agent NaOH solution is subsequently adding and pH is adjusted to 8
~9, obtain the performed polymer aqueous solution of carbamide after being heated to 70 DEG C of reaction 15min;
(2) 0.05g NP-10 and 9g core are mixed, add 2g pH adjusting agents acetic acid and pH is adjusted to 4.5, strong agitation
Under it is fully emulsified;
(3) step product (2) added in step product (1), and insulation is in 65 DEG C of stirrings then molten with pH adjusting agent NaOH
PH is adjusted to 9 by liquid, obtains micro-capsule dispersion liquid;
(4) the product after suction filtration is washed 3 times with formaldehyde, finished product after 30~40 DEG C of dryings.
Embodiment 3
Preparation method is comprised the following steps:
(1) added after 25g polyvinyl alcohol is mixed with 1.5g OP-10 in 50g deionized waters, stirred, add pH to adjust
PH is adjusted to 10 by section agent NaOH solution, obtains water phase;
(2) 10.2g cores are mixed to be dissolved in 50g carbon tetrachloride solutions and obtain organic phase;
(3) strong agitation is fully emulsified after the product by step (1) with step (2) mixes, 50 DEG C of dropwise addition 0.5g ethylenediamines, instead
Answer the microcapsules solidified after 15min.
It is of the invention when using:
Surface of workpiece is cleaned up, and ensures that its surface does not have corrosion, its neat is then placed in casing
It is interior, package vapor phase inhibitor with ventilative gauze and be placed in metal works top, with plastic adhesive tape seal case space, generally use
120~150g/m of amount3, consumption takes the circumstances into consideration to increase under adverse circumstances.
The test of sustained release performance of the invention:
Two parts of the vapour phase inhibitor of phase homogenous quantities is weighed, A parts is not made any treatment, and B parts respectively by the system of embodiment 1,2,3
Preparation Method carries out the microencapsulation of core.A, B sample are respectively placed in after drying 12h in the baking oven of different temperatures and it are weighed, and count
Calculate the percentage that residuals weight accounts for gross weight.
Fig. 1 is the performance comparison of the vapour phase inhibitor by the microencapsulation of embodiment 1 and unencapsulated gas-phase slow-release agent.Figure
2 is the performance comparison of the vapour phase inhibitor by the microencapsulation of embodiment 2 and unencapsulated gas-phase slow-release agent.Fig. 3 is by implementation
The performance comparison of the vapour phase inhibitor of the microencapsulation of example 3 and unencapsulated gas-phase slow-release agent.Exist as can be seen from Figure 1, 2, 3
The vapour phase inhibitor residue percentage of microencapsulation is more than the vapour phase inhibitor of non-microencapsulation, that is, its at identical temperature
With good sustained release performance.
The test of rustless property of the invention
Two parts of the vapour phase inhibitor of phase homogenous quantities is weighed, A parts is not made any treatment, and B parts respectively by the system of embodiment 1,2,3
Preparation Method carries out the microencapsulation of core.A, B sample make the rust-preventing characteristic of vapor phase inhibitor according to method shown in JB/T 6701-92
Can compare, table 1 is the vapour phase inhibitor and the vapour phase inhibitor rustless property pair by the microencapsulation of embodiment 1 of non-microencapsulation
Than.Vapour phase inhibitor of the table 2 for non-microencapsulation and the vapour phase inhibitor rustless property by the microencapsulation of embodiment 2 are contrasted.Table 3
Vapour phase inhibitor for non-microencapsulation and the vapour phase inhibitor rustless property contrast by the microencapsulation of embodiment 3.
Sample | A samples | B samples |
Volatile rust prevention Screening assay | The corrosion of 7 cycles | The corrosion of 9 cycles |
The damp and hot experiment of dynamic Contact | The corrosion of 7 cycles | The corrosion of 10 cycles |
Gas-phase slow-release capacity experimental | It is qualified | It is qualified |
The vapour phase inhibitor of table 1 and microencapsulation antirust agent rustless property are contrasted
Sample | A samples | B samples |
Volatile rust prevention Screening assay | The corrosion of 7 cycles | The corrosion of 10 cycles |
The damp and hot experiment of dynamic Contact | The corrosion of 7 cycles | The corrosion of 10 cycles |
Gas-phase slow-release capacity experimental | It is qualified | It is qualified |
The vapour phase inhibitor of table 2 and microencapsulation antirust agent rustless property are contrasted
Sample | A samples | B samples |
Volatile rust prevention Screening assay | The corrosion of 7 cycles | The corrosion of 9 cycles |
The damp and hot experiment of dynamic Contact | The corrosion of 7 cycles | The corrosion of 10 cycles |
Gas-phase slow-release capacity experimental | It is qualified | It is qualified |
The vapour phase inhibitor of table 3 and microencapsulation antirust agent rustless property are contrasted
A samples are considerably longer than from table 1,2, release time of 3, B samples, for long-distance transport or long-term storage
Metal works can well realize anticorrosion.
In the present invention, the gas-phase slow-release agent of core using octadecane butyl diacid, 1, the alkenyl imidazoline of 2- aminoethyls 17,
The composition of lanolin, BTA and base oil, wall material can be cyanurotriamide modified urea and formaldehyde polymer,
The polymer or polyvinyl alcohol of melamine and formaldehyde, form footpath and are evenly distributed and intensity preferably micro- glue after wall material parcel core
Capsule.When using by microcapsules taken in one's arms with gauze come, be then placed within sealing chest in, microcapsules slowly discharge gas phase delay
Agent is released, each gap in chest can be full of, it is ensured that the metal works safety of storage in it, the speed of release is slow, anti-corrosion
The time of erosion and effect are good, are especially suitable for the anticorrosion of the metal works of long-term transport or long-term storage.The microcapsules of gained
Particle diameter distribution is uniform, and intensity is preferable.
Claims (4)
1. a kind of microencapsulation vapor phase inhibitor, it is characterised in that:Including core and wall material, wall material is wrapped in outside core and forms micro-
Capsule, the core include octadecane butyl diacid, 1, the alkenyl imidazoline of 2- aminoethyls 17, lanolin, BTA and
Base oil, the wall material is synthesis macromolecular material;Also include curing agent and emulsifying agent;
The core includes the following components for mixing by weight percentage:
The core is 1 with the weight ratio of wall material:2~5;
The wall material is that, by the polymer of cyanurotriamide modified urea and formaldehyde, the emulsifying agent is NP-10, vapor phase inhibitor
Preparation method comprise the following steps:
(1) formaldehyde is mixed with urea, heated, pH adjusting agent triethanolamine is then added dropwise pH is adjusted to 8, insulation reaction;
(2) sticky performed polymer is obtained after continuously adding melamine reaction;
(3) NP-10 in core addition deionized water, will be added, insulated and stirred forms uniform tiny dispersed oil droplets;
(4) during the product by step (2) adds step product (3), acetic acid is added dropwise, it is 2.5 to adjust pH, is obtained after reaction micro- after stirring
Capsule dispersant liquid;
(5) the product after suction filtration is washed with formaldehyde, finished product after drying.
2. a kind of microencapsulation vapor phase inhibitor, it is characterised in that:Including core and wall material, wall material is wrapped in outside core and forms micro-
Capsule, the core include octadecane butyl diacid, 1, the alkenyl imidazoline of 2- aminoethyls 17, lanolin, BTA and
Base oil, the wall material is synthesis macromolecular material;Also include curing agent and emulsifying agent;
The core includes the following components for mixing by weight percentage:
The core is 1 with the weight ratio of wall material:2~5;
The wall material is the polymer of melamine and formaldehyde, and the emulsifying agent is NP-10, the preparation method bag of vapor phase inhibitor
Include following steps:
(1) formaldehyde and water are added in melamine, pH adjusting agent NaOH solution is subsequently adding and pH is adjusted to 8~9, heating response
The performed polymer aqueous solution of carbamide is obtained afterwards;
(2) NP-10 and core are mixed, add pH adjusting agent acetic acid and pH is adjusted to 4.5, it is fully emulsified under strong agitation;
(3) step product (1), insulated and stirred are added in step product (2), then pH is adjusted to 9 with NaOH solution, obtain micro-
Capsule dispersant liquid;
(4) washed with formaldehyde after suction filtration, finished product after drying.
3. a kind of microencapsulation vapor phase inhibitor, it is characterised in that:Including core and wall material, wall material is wrapped in outside core and forms micro-
Capsule, the core include octadecane butyl diacid, 1, the alkenyl imidazoline of 2- aminoethyls 17, lanolin, BTA and
Base oil, the wall material is synthesis macromolecular material;Also include curing agent and emulsifying agent;
The core includes the following components for mixing by weight percentage:
The core is 1 with the weight ratio of wall material:2~5;
The wall material is polyvinyl alcohol, and the emulsifying agent is OP-10, and the preparation method of vapor phase inhibitor is comprised the following steps:
(1) added after polyvinyl alcohol is mixed with OP-10 in deionized water, add pH adjusting agent NaOH solution that pH is adjusted to 10, obtained
To water phase;
(2) core is mixed to be dissolved in carbon tetrachloride solution and obtain organic phase;
(3) strong agitation is fully emulsified after the product by step (1) with step (2) mixes, and ethylenediamine is added dropwise, and is solidified after reaction
Microcapsules.
4. a kind of microencapsulation vapor phase inhibitor according to claim 1 or 2 or 3, it is characterised in that:The wall material parcel
Particle diameter after core is 3~100 microns.
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CN110863203A (en) * | 2019-07-31 | 2020-03-06 | 泰伦特生物工程股份有限公司 | Slow-release gas-phase antirust agent and preparation method thereof |
CN111088496A (en) * | 2019-11-25 | 2020-05-01 | 刘振国 | Microcapsule for gas-phase anti-rust film |
CN112725806B (en) * | 2020-12-29 | 2023-03-21 | 宁德师范学院 | Neodymium-iron-boron composite corrosion inhibitor and application thereof |
CN115584506B (en) * | 2021-07-05 | 2024-04-16 | 天津科技大学 | Preparation method of green efficient compound gas phase corrosion inhibitor for carbon steel |
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CN102392253A (en) * | 2011-11-25 | 2012-03-28 | 深圳大学 | Polyacrylic acid type calcium nitrite corrosion inhibitor and preparation method thereof |
CN102719302A (en) * | 2012-07-03 | 2012-10-10 | 上海福岛化工科技发展有限公司 | Volatile rust preventive oil |
CN102977982A (en) * | 2012-10-31 | 2013-03-20 | 铜陵瑞莱科技有限公司 | Ammonium benzoate gas-phase slow-release rust preventive oil and preparation method thereof |
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CN85102059A (en) * | 1985-04-01 | 1986-09-17 | 中国石油化工总公司兰州炼油厂 | Oil engine is sealed up for safekeeping and the lubricated oil additives plural components of trial trip |
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