CN107793901A - A kind of production method for the poly-aspartate polyurea water-proof corrosion-inhibiting coating that graphene is modified - Google Patents
A kind of production method for the poly-aspartate polyurea water-proof corrosion-inhibiting coating that graphene is modified Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/02—Polyureas
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/60—Polyamides or polyester-amides
- C08G18/603—Polyamides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Paints Or Removers (AREA)
Abstract
The poly-aspartate polyurea water-proof corrosion-inhibiting coating that a kind of graphene is modified, it is characterised in that prepare graphene oxide first；Secondly, modification is carried out to graphene oxide by IPDI and phenylhydrazine reduces to it, isocyanate-modified graphene is prepared；Then, aspartate is obtained by mikey addition by di-2-ethylhexyl maleate and ethylenediamine；Finally using aspartate as raw material, HDI is curing agent, and isocyanate-modified graphene is modifying agent, is aided with other auxiliary agents and is mixed with coating, is applied, and is solidified, and maintenance, obtains the poly-aspartate polyurea water-proof corrosion-inhibiting coating of graphene modification.Water-tight corrosion-proof coating provided by the invention, had both saved the excellent properties of traditional carbamide paint, while it is too fast, it is necessary to the drawbacks of Special Equipment is constructed to overcome traditional polyurea gel time again.
Description
Technical field
The present invention relates to a kind of corrosion-inhibiting coating, the poly-aspartate polyurea water-proof anti-corrosion that especially a kind of graphene is modified applies
The production method of layer.
Background technology
Polyurea coating has the following advantages that compared with traditional environment-friendly materials：Catalyst need not be added, is had higher
Reaction speed, can quickly solidify, can the spray mo(u)lding on any vertical plane, inclined-plane and curved surface, be not in sagging
Phenomenon, gel time is short, with regard to that can reach walking intensity in a few minutes；It is insensitive to temperature, moisture and moisture, during construction not by
The influence of humidity, environment temperature and construction parts；It is two-component system, solid content 100%, without other volatility
Organic matter, it is free from environmental pollution, be not in the peculiar smell caused by solvent volatilization during construction.
It is very short yet with its gel time, the time of only several seconds, so traditional spray polyurea coating construction must
Special HTHP impacting type mixing apparatus must be used, this not only increases construction cost, is unfavorable for general workmen's again
Operation.
The content of the invention
It is an object of the invention to provide the poly-aspartate polyurea water-proof that a kind of rational graphene of gel time is modified
The production method of corrosion-inhibiting coating.
To achieve these goals, present invention employs following technical scheme：
The poly-aspartate polyurea water-proof corrosion-inhibiting coating that a kind of graphene is modified, it is characterised in that prepare graphene oxide first；
Secondly, modification is carried out to graphene oxide by IPDI and phenylhydrazine reduces to it, be prepared different
Cyanate modified graphene；Then, polyaspartate is obtained by mikey addition by di-2-ethylhexyl maleate and ethylenediamine；
Finally using polyaspartate as raw material, HDI is curing agent, and isocyanate-modified graphene is modifying agent, is aided with other auxiliary agents
Coating is mixed with, is applied, is solidified, maintenance, obtains the poly-aspartate polyurea water-proof corrosion-inhibiting coating of graphene modification.
The poly-aspartate polyurea water-proof corrosion-inhibiting coating that described graphene is modified, it is characterised in that it has the following steps
It is prepared：
（1）Reaction vessel is placed in ice-water bath, sequentially adds natural flake graphite, sodium nitrate and the concentrated sulfuric acid, is well mixed, stirs
After mixing 20-30min, 3-4 addition potassium permanganate of part, interval 30min is added every time, after addition, continues magnetic agitation 2-
3h, rise temperature continue temperature constant magnetic stirring 3-4h, deionized water are added dropwise, controls and is dripped in 1-1.5h to 35-40 DEG C
Finish, be cooled to room temperature, add 30% hydrogen peroxide, stand 20-24h, filtering, washed 5-6 times using 5% hydrochloric acid solution；Will
Gained material is centrifuged repeatedly washing to supernatant to neutrality using deionized water again, leaving layer colloid, is placed in 35-40 DEG C of vacuum and does
Dried in dry case, obtain graphene oxide；
（2）Graphene oxide and DMF are added in reaction vessel, the ultrasonic 1.5-2h under 200-250W ultrasonic power, turned
Move in 80-85 DEG C of water-bath, add IPDI, temperature constant magnetic stirring reaction 4-6h, reduce temperature to 60-
65 DEG C, phenylhydrazine is added, continues temperature constant magnetic stirring reaction 4-6h, temperature is reduced to room temperature, filtering, 2- is washed using dichloromethane
3 times, it is placed in 35-40 DEG C of vacuum drying chamber and dries, obtain isocyanate-modified graphene；
（3）By hexamethylene diamine be added to agitator, thermometer, reflux condensing tube reaction vessel in, start stirring, and be passed through
Nitrogen, and keeping temperature is 40-50 DEG C, after hexamethylene diamine thawing, starts that di-2-ethylhexyl maleate is added dropwise, controls and dripped in 2-3h
Finish, be warming up to 60-65 DEG C, temperature constant magnetic stirring reaction 6-8h, obtain polyaspartate；
（4）Polyaspartate, hexamethylene diisocyanate, isocyanate-modified graphene are added in material-compound tank, mixed
Conjunction stirs, and adds dispersant SK-5040 and defoamer PA-311, continues to stir, even application in working interface,
Spontaneous curing, room temperature maintenance 5-6d, obtains the poly-aspartate polyurea water-proof corrosion-inhibiting coating of graphene modification.
The preparation method for the poly-aspartate polyurea water-proof corrosion-inhibiting coating that described graphene is modified, it is characterised in that step
Suddenly（1）Middle natural flake graphite, sodium nitrate, the concentrated sulfuric acid, potassium permanganate, the mass ratio of deionized water and 30% hydrogen peroxide are
1：0.48-0.52：25-30：2.8-3.2：30-35：4-5.
The preparation method for the poly-aspartate polyurea water-proof corrosion-inhibiting coating that described graphene is modified, it is characterised in that step
Suddenly（2）Middle graphene oxide, DMF, the mass ratio of IPDI and phenylhydrazine are 1：120-150：8-8.5：4-
4.5。
The preparation method for the poly-aspartate polyurea water-proof corrosion-inhibiting coating that described graphene is modified, it is characterised in that step
Suddenly（3）The mass ratio of middle hexamethylene diamine and di-2-ethylhexyl maleate is 1：2-2.2
The preparation method for the poly-aspartate polyurea water-proof corrosion-inhibiting coating that described graphene is modified, it is characterised in that step（4）
Middle winter propylhomoserin ester, hexamethylene diisocyanate, isocyanate-modified graphene, dispersant SK-5040 and defoamer PA-311
Mass ratio be 1：1-1.05：0.08-0.1：0.002-0.003：0.001-0.002.
By using above-mentioned technical scheme, the present invention has the advantages that：
The method comprises the steps of firstly, preparing graphene oxide；Then modification is carried out to graphene oxide by IPDI to change
Property and phenylhydrazine reduce to it, and isocyanate-modified graphene is prepared；The finally isocyanate-modified stone to be prepared
Black alkene is modifying agent, and isocyanates can participate in polyaspartate and HDI reaction in isocyanate-modified graphene, is increased
Add the compatibility of graphene and polyureas, improve the degree of scatter of graphene in the coating；Graphene tends to parallel to coating simultaneously
Surface alignment, one layer of inert, resist chemical protective layer is formd, make it that air and moisture can be prevented to enter, can also prevent
Only coating stress, which is concentrated, produces cracking, improves the critical film Cracking Thickness of coating.The present invention passes through di-2-ethylhexyl maleate and second
Diamines obtains polyaspartate by mikey addition；Primary amine is converted into secondary amine in the course of reaction of polyaspartate, by
In space steric effect, the reaction speed of polyaspartate and isocyanate groups is reduced, the polyurea coating of preparation has
Preferable mobility and levelability；Both the excellent properties of traditional carbamide paint had been saved, while have overcome traditional polyurea gel again
Time is too fast, it is necessary to the drawbacks of Special Equipment is constructed.The coating of the present invention has adhesive force is strong, good toughness, wear-resisting
The advantages that performance, weather resistance are good, and without solvent, it is green, once spraying i.e. can reach required thickness.
Embodiment
The poly-aspartate polyurea water-proof corrosion-inhibiting coating that the graphene of the present embodiment is modified, its have the following steps preparation and
Into：
（1）Reaction vessel is placed in ice-water bath, sequentially adds natural flake graphite, sodium nitrate and the concentrated sulfuric acid, is well mixed, stirs
After mixing 30min, 3 addition potassium permanganate of part, interval 30min is added every time, after addition, continues magnetic agitation 3h, rise
Temperature continues temperature constant magnetic stirring 4h, deionized water is added dropwise, controls and is added dropwise in 1.5h, is cooled to room temperature to 40 DEG C,
30% hydrogen peroxide is added, 24h is stood, filtering, is washed 6 times using 5% hydrochloric acid solution；Gained material is used into deionization again
Water is centrifuged repeatedly washing to supernatant to neutrality, leaving layer colloid, is placed in 40 DEG C of vacuum drying chambers and dries, obtain graphite oxide
Alkene；
（2）Graphene oxide and DMF are added in reaction vessel, the ultrasonic 2h under 250W ultrasonic power, are transferred to 85 DEG C
In water-bath, IPDI is added, temperature constant magnetic stirring reaction 6h, temperature is reduced to 65 DEG C, adds phenylhydrazine, after
Continuous temperature constant magnetic stirring reaction 6h, temperature is reduced to room temperature, filtering, is washed 3 times using dichloromethane, is placed in 40 DEG C of vacuum drying
Dried in case, obtain isocyanate-modified graphene；
（3）By hexamethylene diamine be added to agitator, thermometer, reflux condensing tube reaction vessel in, start stirring, and be passed through
Nitrogen, and keeping temperature is 50 DEG C, after hexamethylene diamine thawing, starts that di-2-ethylhexyl maleate is added dropwise, controls and be added dropwise in 3h, rise
Temperature temperature constant magnetic stirring reaction 8h, obtains polyaspartate to 65 DEG C；
（4）Polyaspartate, hexamethylene diisocyanate, isocyanate-modified graphene are added in material-compound tank, mixed
Conjunction stirs, and adds dispersant SK-5040 and defoamer PA-311, continues to stir, even application in working interface,
Spontaneous curing, room temperature maintenance 6d, obtains the poly-aspartate polyurea water-proof corrosion-inhibiting coating of graphene modification.
The step of the present embodiment（1）Middle natural flake graphite, sodium nitrate, the concentrated sulfuric acid, potassium permanganate, deionized water and 30%
Hydrogen peroxide mass ratio be 1：0.5：30：3：35：5.
The step of the present embodiment（2）Middle graphene oxide, DMF, the mass ratio of IPDI and phenylhydrazine are
1：150：8.5：4.5.
The step of the present embodiment（3）The mass ratio of middle hexamethylene diamine and di-2-ethylhexyl maleate is 1：2.1
The step of the present embodiment（4）Middle winter propylhomoserin ester, hexamethylene diisocyanate, isocyanate-modified graphene, dispersant
SK-5040 and defoamer PA-311 mass ratio are 1：1.05：0.1：0.003：0.002.
Claims (6)
1. the poly-aspartate polyurea water-proof corrosion-inhibiting coating that a kind of graphene is modified, it is characterised in that prepare graphite oxide first
Alkene；Secondly, modification is carried out to graphene oxide by IPDI and phenylhydrazine reduces to it, be prepared
Isocyanate-modified graphene；Then, poly-aspartate is obtained by mikey addition by di-2-ethylhexyl maleate and ethylenediamine
Ester；Finally using polyaspartate as raw material, HDI is curing agent, and isocyanate-modified graphene is modifying agent, is aided with other and helps
Agent is mixed with coating, applies, and solidifies, and maintenance, obtains the poly-aspartate polyurea water-proof corrosion-inhibiting coating of graphene modification.
2. the poly-aspartate polyurea water-proof corrosion-inhibiting coating that graphene according to claim 1 is modified, it is characterised in that its
Have the following steps and be prepared：
（1）Reaction vessel is placed in ice-water bath, sequentially adds natural flake graphite, sodium nitrate and the concentrated sulfuric acid, is well mixed, stirs
After mixing 20-30min, 3-4 addition potassium permanganate of part, interval 30min is added every time, after addition, continues magnetic agitation 2-
3h, rise temperature continue temperature constant magnetic stirring 3-4h, deionized water are added dropwise, controls and is dripped in 1-1.5h to 35-40 DEG C
Finish, be cooled to room temperature, add 30% hydrogen peroxide, stand 20-24h, filtering, washed 5-6 times using 5% hydrochloric acid solution；Will
Gained material is centrifuged repeatedly washing to supernatant to neutrality using deionized water again, leaving layer colloid, is placed in 35-40 DEG C of vacuum and does
Dried in dry case, obtain graphene oxide；
（2）Graphene oxide and DMF are added in reaction vessel, the ultrasonic 1.5-2h under 200-250W ultrasonic power, turned
Move in 80-85 DEG C of water-bath, add IPDI, temperature constant magnetic stirring reaction 4-6h, reduce temperature to 60-
65 DEG C, phenylhydrazine is added, continues temperature constant magnetic stirring reaction 4-6h, temperature is reduced to room temperature, filtering, 2- is washed using dichloromethane
3 times, it is placed in 35-40 DEG C of vacuum drying chamber and dries, obtain isocyanate-modified graphene；
（3）By hexamethylene diamine be added to agitator, thermometer, reflux condensing tube reaction vessel in, start stirring, and be passed through
Nitrogen, and keeping temperature is 40-50 DEG C, after hexamethylene diamine thawing, starts that di-2-ethylhexyl maleate is added dropwise, controls and dripped in 2-3h
Finish, be warming up to 60-65 DEG C, temperature constant magnetic stirring reaction 6-8h, obtain polyaspartate；
（4）Polyaspartate, hexamethylene diisocyanate, isocyanate-modified graphene are added in material-compound tank, mixed
Conjunction stirs, and adds dispersant SK-5040 and defoamer PA-311, continues to stir, even application in working interface,
Spontaneous curing, room temperature maintenance 5-6d, obtains the poly-aspartate polyurea water-proof corrosion-inhibiting coating of graphene modification.
3. the preparation method for the poly-aspartate polyurea water-proof corrosion-inhibiting coating that graphene according to claim 2 is modified, its
It is characterised by, step（1）Middle natural flake graphite, sodium nitrate, the concentrated sulfuric acid, potassium permanganate, deionized water and 30% hydrogen peroxide
Mass ratio be 1：0.48-0.52：25-30：2.8-3.2：30-35：4-5.
4. the preparation method for the poly-aspartate polyurea water-proof corrosion-inhibiting coating that graphene according to claim 2 is modified, its
It is characterised by, step（2）Middle graphene oxide, DMF, the mass ratio of IPDI and phenylhydrazine are 1：120-150：
8-8.5：4-4.5.
5. the preparation method for the poly-aspartate polyurea water-proof corrosion-inhibiting coating that graphene according to claim 2 is modified, its
It is characterised by, step（3）The mass ratio of middle hexamethylene diamine and di-2-ethylhexyl maleate is 1：2-2.2.
6. the preparation method for the poly-aspartate polyurea water-proof corrosion-inhibiting coating that graphene according to claim 2 is modified, its
It is characterised by, step（4）Middle winter propylhomoserin ester, hexamethylene diisocyanate, isocyanate-modified graphene, dispersant SK-
5040 and defoamer PA-311 mass ratio is 1：1-1.05：0.08-0.1：0.002-0.003：0.001-0.002.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108373812A (en) * | 2018-03-26 | 2018-08-07 | 湖南科技大学 | A kind of preparation method of the aqueous polyureas graft grapheme coating material of the anti-albumen of anticorrosion and antifouling |
| CN108584928A (en) * | 2018-05-30 | 2018-09-28 | 谢新昇 | A kind of preparation method of graphene heat conducting film |
| CN108642499A (en) * | 2018-05-18 | 2018-10-12 | 赵建平 | A kind of preparation method of rust remover |
| CN109135526A (en) * | 2018-07-20 | 2019-01-04 | 成都上泰科技有限公司 | A kind of synthesis technology of epoxidized soybean oil modified polyaspartic acid ester polyurea copolymers |
| CN110922871A (en) * | 2019-11-24 | 2020-03-27 | 湖南科技大学 | Preparation method of hydrophobic polyurea/graphene oxide protective coating material and product thereof |
| CN111410905A (en) * | 2020-04-26 | 2020-07-14 | 朱建程 | Functional graphene modified polyurethane conductive anticorrosive coating and preparation method thereof |
| CN109266187B (en) * | 2018-08-10 | 2021-02-05 | 恒力盛泰（厦门）石墨烯科技有限公司 | Heat dissipation coating containing isocyanate modified graphene and preparation method thereof |
| CN116355509A (en) * | 2023-03-14 | 2023-06-30 | 江苏大学 | Anti-aging low-adhesion composite coating with sea wear applicability, preparation method and application |
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| CN111410905A (en) * | 2020-04-26 | 2020-07-14 | 朱建程 | Functional graphene modified polyurethane conductive anticorrosive coating and preparation method thereof |
| CN116355509A (en) * | 2023-03-14 | 2023-06-30 | 江苏大学 | Anti-aging low-adhesion composite coating with sea wear applicability, preparation method and application |
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Application publication date: 20180313 |