CN104388944A - Microencapsulated vapor phase rust inhibitor and preparation method thereof - Google Patents
Microencapsulated vapor phase rust inhibitor and preparation method thereof Download PDFInfo
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- CN104388944A CN104388944A CN201410728957.8A CN201410728957A CN104388944A CN 104388944 A CN104388944 A CN 104388944A CN 201410728957 A CN201410728957 A CN 201410728957A CN 104388944 A CN104388944 A CN 104388944A
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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
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Abstract
The invention relates to a microencapsulated vapor phase rust inhibitor which comprises the following raw materials: zinc dihydrogen phosphate, manganous dihydrogen phosphate, nickel nitrate, sodium fluoride, sodium nitrate, phosphoric acid, citric acid, phosphotungstic acid and sodium molybdate. According to the microencapsulated vapor phase rust inhibitor disclosed by the invention, the components are mixed with deionized water so as to prepare the finished product. The rust inhibitor is used according to the following steps: putting a NdFeB magnetic material into an ultrasonic roller, treating according to a sequence of oil removal, cleaning, surface conditioning, treatment by using special surface treating agents for NdFeB, closing and drying, so that the micro rust can be removed from the surface at first and then a uniform and dense protective film is formed on the surface, wherein the weight loss of the treated NdFeB magnetic material is small. The saline soaking test proves that the vapor phase rust inhibitor is corrosion-resistant, and hazards of strong acid pickling to the environment and operators are reduced.
Description
Technical field
The invention belongs to metal products technical field of rust prevention, especially a kind of micro encapsulation vapor phase inhibitor and preparation method thereof.
Background technology
The harm that metal products can be got rusty in shipping storage process, its major cause is relative humidity of atomsphere, temperature and humidity, corrosive gases and other corrosion factor, people more often adopt top layer brushing Erosion-Resisting Non-metallic Materials, top layer plates corrosion resistant metal, chemical process forms the methods such as sull, along with the development of science and technology, vapor phase inhibitor technology more and more welcomed by the people, it is through special synthesis technique, the composite a kind of corrosion inhibitor be prepared from, separately or suitable carrier can be depended on, direct gasification at normal temperatures and pressures, can be full of in sealed environment in any spatial gaps, and be adsorbed on metallic surface, form very thin fine and close protective film, effective exclusion of water, oxygen and other corrosion factors, suppress the electrochemical reaction impelling metallic corrosion, thus reach best rust protection effect.
Because vapour-phase inhibitor release sustained-release particle degree of freedom is high, so its release rate is uncontrollable, causes the shortcoming that vapour-phase inhibitor life cycle is short, usage quantity is large thus, bring negative impact to national economy and environment.As can be seen here, how to reduce the release rate of inhibiter, extend inhibiter life cycle, control it and use total amount to be an important problem, not only saved use cost but also be conducive to preserving the ecological environment.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, scientific matching, slowly-releasing and a kind of micro encapsulation vapor phase inhibitor of favorable rust preventing effect are provided.
The technical scheme that the present invention takes is:
A kind of micro encapsulation vapor phase inhibitor, it is characterized in that: comprise core and wall material, wall material is wrapped in core and forms microcapsule outward, described core comprise octadecane butyl diacid, 1,2-aminoethyl 17 alkenyl imidazoline, lanolin, benzotriazole and base oil, described wall material is synthesized polymer material.
And, also comprise solidifying agent and emulsifying agent.
And described core comprises the following component mixed by weight percentage:
The weight ratio of described core and wall material is 1:2 ~ 5.
And described wall material is by the cyanurotriamide modified polymkeric substance obtaining urea and formaldehyde.
And described wall material is the polymkeric substance of trimeric cyanamide and formaldehyde.
And described wall material is polyvinyl alcohol.
Another object of the present invention is to provide a kind of preparation method of micro encapsulation vapor phase inhibitor, it is characterized in that: comprise the following steps:
(1) formaldehyde is mixed with urea, heating, then drip pH adjusting agent and pH is adjusted to 8, insulation reaction;
(2) after continuing to add trimeric cyanamide reaction, obtain thickness performed polymer;
(3) core is added in deionized water, then add NP-10, insulated and stirred, form evenly tiny dispersed oil droplets;
(4) step product is (2) added in step product (3), after stirring, drip acetic acid, adjust pH to be 2.5, after reaction, obtain micro-capsule dispersion liquid;
(5) the product formaldehyde after suction filtration washs, obtained finished product after dry.
Another object of the present invention is to provide a kind of preparation method of micro encapsulation vapor phase inhibitor, it is characterized in that: comprise the following steps:
(1) in trimeric cyanamide, add formaldehyde and water, then add pH adjusting agent and pH is adjusted to 8 ~ 9, after reacting by heating, obtain the performed polymer aqueous solution of carbamide;
(2) by NP-10 and core mixing, then add pH adjusting agent pH is adjusted to 4.5, fully emulsified under violent stirring;
(3) in step product (2), add step product (1), insulated and stirred, then by pH adjusting agent, pH is adjusted to 9, obtain micro-capsule dispersion liquid;
(4) wash with formaldehyde after suction filtration, obtained finished product after dry.
Another object of the present invention is to provide a kind of preparation method of micro encapsulation vapor phase inhibitor, it is characterized in that: comprise the following steps:
(1) add after polyvinyl alcohol being mixed with OP-10 in deionized water, add pH adjusting agent and pH is adjusted to 10, obtain aqueous phase;
(2) core mixing is dissolved in carbon tetrachloride solution and obtains organic phase;
(3) step is (1) fully emulsified with the step rear violent stirring of product mixing (2), drip quadrol, after reaction, obtain the microcapsule solidified.
And the particle diameter after described wall material parcel core is 3 ~ 100 microns.
Advantage of the present invention and positively effect are:
In the present invention, the gas-phase slow-release agent of core use octadecane butyl diacid, 1,2-aminoethyl 17 alkenyl imidazoline, lanolin, benzotriazole and base oil composition, wall material can be polymkeric substance or the polyvinyl alcohol of the polymkeric substance of cyanurotriamide modified urea and formaldehyde, trimeric cyanamide and formaldehyde, forms footpath and be evenly distributed and the good microcapsule of intensity after wall material parcel core.During use, microcapsule gauze is taken in one's arms, then be placed in the chest of sealing, microcapsule discharge gas-phase slow-release agent slowly, the each gap in chest can be full of, ensure the metal works safety deposited in it, the speed of release is slow, etch-proof time and effective, is especially applicable to the protection against corrosion of the metal works of long-term transport or long-term storage.The Microcapsules Size of gained is evenly distributed, and intensity is better.
Accompanying drawing explanation
Fig. 1 is embodiment 1 and not encapsulated gas-phase slow-release agent corrosion inhibition comparison diagram;
Fig. 2 is embodiment 2 and not encapsulated gas-phase slow-release agent corrosion inhibition comparison diagram;
Fig. 3 is embodiment 3 and not encapsulated gas-phase slow-release agent corrosion inhibition comparison diagram;
Fig. 4 is the stereoscan photograph of microcapsule.
Embodiment
Below in conjunction with embodiment, the present invention is further described, and following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
A kind of micro encapsulation vapor phase inhibitor, innovation of the present invention is: comprise core and wall material, wall material is wrapped in core and forms microcapsule outward, described core comprise octadecane butyl diacid, 1,2-aminoethyl 17 alkenyl imidazoline, lanolin, benzotriazole and base oil, described wall material is synthesized polymer material.
Solidifying agent and emulsifying agent is also comprised in said components.Wherein core comprises the following component mixed by weight percentage:
Core and wall material weight ratio are therebetween 1:2 ~ 5.
Wall material is macromolecular material, can be following three kinds of components, specifically: 1. the cyanurotriamide modified polymkeric substance obtaining urea and formaldehyde, the 2. polymkeric substance of trimeric cyanamide and formaldehyde, 3. polyvinyl alcohol.
If wall material is 1, then the preparation method of micro encapsulation vapor phase inhibitor comprises the following steps:
(1) formaldehyde is mixed with urea, heating, then drip pH adjusting agent and pH is adjusted to 8, insulation reaction;
(2) after continuing to add trimeric cyanamide reaction, obtain thickness performed polymer;
(3) core is added in deionized water, then add NP-10, insulated and stirred, form evenly tiny dispersed oil droplets;
(4) step product is (2) added in step product (3), after stirring, drip acetic acid, adjust pH to be 2.5, after reaction, obtain micro-capsule dispersion liquid;
(5) the product formaldehyde after suction filtration washs, obtained finished product after dry.
If wall material is 2, then the preparation method of micro encapsulation vapor phase inhibitor, it is characterized in that: comprise the following steps:
(1) in trimeric cyanamide, add formaldehyde and water, then add pH adjusting agent and pH is adjusted to 8 ~ 9, after reacting by heating, obtain the performed polymer aqueous solution of carbamide;
(2) by NP-10 and core mixing, then add pH adjusting agent pH is adjusted to 4.5, fully emulsified under violent stirring;
(3) in step product (2), add step product (1), insulated and stirred, then by pH adjusting agent, pH is adjusted to 9, obtain micro-capsule dispersion liquid;
(4) wash with formaldehyde after suction filtration, obtained finished product after dry.
If wall material is 3, then the preparation method of micro encapsulation vapor phase inhibitor, it is characterized in that: comprise the following steps:
(1) add after polyvinyl alcohol being mixed with OP-10 in deionized water, add pH adjusting agent and pH is adjusted to 10, obtain aqueous phase;
(2) core mixing is dissolved in carbon tetrachloride solution and obtains organic phase;
(3) step is (1) fully emulsified with the step rear violent stirring of product mixing (2), drip quadrol, after reaction, obtain the microcapsule solidified.
No matter which kind of method prepares the microcapsule that wall material wraps up core, and the particle diameter of these microcapsule is between 3 ~ 100 microns.
Embodiment 1
Preparation method comprises the following steps:
(1) 10.2g formaldehyde is mixed with 24.3g urea, be heated to 70 DEG C, then drip pH adjusting agent trolamine and pH is adjusted to 8, insulation reaction 1h;
(2) continue to add 30g trimeric cyanamide, after stirring reaction 1h, obtain thickness performed polymer;
(3) 20g core is added in 100ml deionized water, then add 0.05g NP-10, keep temperature 35 DEG C to stir 30min, form evenly tiny dispersed oil droplets;
(4) added in step product (3) by step product (2), adding speed is 0.5ml/min, drips acetic acid 2.0g after stirring 1h, adjusts pH to be 2.5, obtains micro-capsule dispersion liquid after reaction 1h;
(5) the product formaldehyde after suction filtration washs 3 times, 30 ~ 40 DEG C of dryings obtained finished product afterwards.
Embodiment 2
Preparation method comprises the following steps:
(1) in 10g trimeric cyanamide, add 15g formaldehyde and 25g water, then add pH adjusting agent NaOH solution and pH is adjusted to 8 ~ 9, after being heated to 70 DEG C of reaction 15min, obtain the performed polymer aqueous solution of carbamide;
(2) by 0.05g NP-10 and the mixing of 9g core, then add 2g pH adjusting agent acetic acid pH is adjusted to 4.5, fully emulsified under violent stirring;
(3) in step product (1), add step product (2), be incubated 65 DEG C of stirrings, then by pH adjusting agent NaOH solution, pH be adjusted to 9, obtain micro-capsule dispersion liquid;
(4) the product formaldehyde after suction filtration washs 3 times, 30 ~ 40 DEG C of dryings obtained finished product afterwards.
Embodiment 3
Preparation method comprises the following steps:
(1) add in 50g deionized water after 25g polyvinyl alcohol being mixed with 1.5g OP-10, stir, add pH adjusting agent NaOH solution and pH is adjusted to 10, obtain aqueous phase;
(2) the mixing of 10.2g core is dissolved in 50g carbon tetrachloride solution and obtains organic phase;
(3) step is (1) fully emulsified with the step rear violent stirring of product mixing (2), 50 DEG C drip 0.5g quadrols, obtain the microcapsule solidified after reaction 15min.
During use of the present invention:
Surface of workpiece is cleaned up, and guarantees that its surface does not have corrosion, then it neat is put in casing, package vapor phase inhibitor with ventilative gauze and be placed in metal works top, with plastic adhesive tape seal case space, general usage quantity 120 ~ 150g/m
3, under severe environment, consumption takes the circumstances into consideration to increase.
The test of sustained release performance of the present invention:
Take the vapour-phase inhibitor two parts of equal in quality, A part does not do any process, and B part carries out the micro encapsulation of core respectively by the preparation method of embodiment 1,2,3.A, B sample is weighed to it after being positioned over respectively and drying 12h in the baking oven of differing temps, calculates the per-cent that residuals weight accounts for gross weight.
Fig. 1 is vapour-phase inhibitor by embodiment 1 micro encapsulation and the performance comparison of not encapsulated gas-phase slow-release agent.Fig. 2 is vapour-phase inhibitor by embodiment 2 micro encapsulation and the performance comparison of not encapsulated gas-phase slow-release agent.Fig. 3 is vapour-phase inhibitor by embodiment 3 micro encapsulation and the performance comparison of not encapsulated gas-phase slow-release agent.The vapour-phase inhibitor residuum per-cent of micro encapsulation is more than the vapour-phase inhibitor of non-micro encapsulation at the same temperature as can be seen from Figure 1, 2, 3, and namely it has good sustained release performance.
The test of rustless property of the present invention
Take the vapour-phase inhibitor two parts of equal in quality, A part does not do any process, and B part carries out the micro encapsulation of core respectively by the preparation method of embodiment 1,2,3.The rustless property that A, B sample makes vapor phase inhibitor according to method shown in JB/T 6701-92 compares, and table 1 is the vapour-phase inhibitor of non-micro encapsulation and contrasts by the vapour-phase inhibitor rustless property of embodiment 1 micro encapsulation.Table 2 is the vapour-phase inhibitor of non-micro encapsulation and contrasts by the vapour-phase inhibitor rustless property of embodiment 2 micro encapsulation.Table 3 is the vapour-phase inhibitor of non-micro encapsulation and contrasts by the vapour-phase inhibitor rustless property of embodiment 3 micro encapsulation.
| Sample | A sample | B sample |
| 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 | Qualified | Qualified |
Table 1 vapour-phase inhibitor and the contrast of micro encapsulation rust-preventive agent rustless property
| Sample | A sample | B sample |
| 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 | Qualified | Qualified |
Table 2 vapour-phase inhibitor and the contrast of micro encapsulation rust-preventive agent rustless property
| Sample | A sample | B sample |
| 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 | Qualified | Qualified |
Table 3 vapour-phase inhibitor and the contrast of micro encapsulation rust-preventive agent rustless property
From table 1,2, time of releasing of 3, B samples be obviously longer than A sample, the metal works for long-distance transport or long-term storage all well can realize protection against corrosion.
In the present invention, the gas-phase slow-release agent of core use octadecane butyl diacid, 1,2-aminoethyl 17 alkenyl imidazoline, lanolin, benzotriazole and base oil composition, wall material can be polymkeric substance or the polyvinyl alcohol of the polymkeric substance of cyanurotriamide modified urea and formaldehyde, trimeric cyanamide and formaldehyde, forms footpath and be evenly distributed and the good microcapsule of intensity after wall material parcel core.During use, microcapsule gauze is taken in one's arms, then be placed in the chest of sealing, microcapsule discharge gas-phase slow-release agent slowly, the each gap in chest can be full of, ensure the metal works safety deposited in it, the speed of release is slow, etch-proof time and effective, is especially applicable to the protection against corrosion of the metal works of long-term transport or long-term storage.The Microcapsules Size of gained is evenly distributed, and intensity is better.
Claims (10)
1. a micro encapsulation vapor phase inhibitor, it is characterized in that: comprise core and wall material, wall material is wrapped in core and forms microcapsule outward, described core comprise octadecane butyl diacid, 1,2-aminoethyl 17 alkenyl imidazoline, lanolin, benzotriazole and base oil, described wall material is synthesized polymer material.
2. a kind of micro encapsulation vapor phase inhibitor according to claim 1, is characterized in that: also comprise solidifying agent and emulsifying agent.
3. a kind of micro encapsulation vapor phase inhibitor according to claim 2, is characterized in that: described core comprises the following component mixed by weight percentage:
The weight ratio of described core and wall material is 1:2 ~ 5.
4. a kind of micro encapsulation vapor phase inhibitor according to claim 3, is characterized in that: described wall material is by the cyanurotriamide modified polymkeric substance obtaining urea and formaldehyde.
5. a kind of micro encapsulation vapor phase inhibitor according to claim 3, is characterized in that: described wall material is the polymkeric substance of trimeric cyanamide and formaldehyde.
6. a kind of micro encapsulation vapor phase inhibitor according to claim 3, is characterized in that: described wall material is polyvinyl alcohol.
7. the preparation method of a kind of micro encapsulation vapor phase inhibitor according to claim 4, is characterized in that: comprise the following steps:
(1) formaldehyde is mixed with urea, heating, then drip pH adjusting agent and pH is adjusted to 8, insulation reaction;
(2) after continuing to add trimeric cyanamide reaction, obtain thickness performed polymer;
(3) core is added in deionized water, then add NP-10, insulated and stirred, form evenly tiny dispersed oil droplets;
(4) step product is (2) added in step product (3), after stirring, drip acetic acid, adjust pH to be 2.5, after reaction, obtain micro-capsule dispersion liquid;
(5) the product formaldehyde after suction filtration washs, obtained finished product after dry.
8. the preparation method of a kind of micro encapsulation vapor phase inhibitor according to claim 5, is characterized in that: comprise the following steps:
(1) in trimeric cyanamide, add formaldehyde and water, then add pH adjusting agent and pH is adjusted to 8 ~ 9, after reacting by heating, obtain the performed polymer aqueous solution of carbamide;
(2) by NP-10 and core mixing, then add pH adjusting agent pH is adjusted to 4.5, fully emulsified under violent stirring;
(3) in step product (2), add step product (1), insulated and stirred, then by pH adjusting agent, pH is adjusted to 9, obtain micro-capsule dispersion liquid;
(4) wash with formaldehyde after suction filtration, obtained finished product after dry.
9. the preparation method of a kind of micro encapsulation vapor phase inhibitor according to claim 6, is characterized in that: comprise the following steps:
(1) add after polyvinyl alcohol being mixed with OP-10 in deionized water, add pH adjusting agent and pH is adjusted to 10, obtain aqueous phase;
(2) core mixing is dissolved in carbon tetrachloride solution and obtains organic phase;
(3) step is (1) fully emulsified with the step rear violent stirring of product mixing (2), drip quadrol, after reaction, obtain the microcapsule solidified.
10. a kind of micro encapsulation vapor phase inhibitor according to claim 2,3,4,5,6,7,8 or 9, is characterized in that: the particle diameter after described wall material parcel core is 3 ~ 100 microns.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN112725806A (en) * | 2020-12-29 | 2021-04-30 | 宁德师范学院 | Neodymium-iron-boron composite corrosion inhibitor and application thereof |
| CN115584506A (en) * | 2021-07-05 | 2023-01-10 | 天津科技大学 | Preparation method of green efficient compound vapor phase corrosion inhibitor for carbon steel |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112725806A (en) * | 2020-12-29 | 2021-04-30 | 宁德师范学院 | Neodymium-iron-boron composite corrosion inhibitor and application thereof |
| CN115584506A (en) * | 2021-07-05 | 2023-01-10 | 天津科技大学 | Preparation method of green efficient compound vapor phase corrosion inhibitor for carbon steel |
| 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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