CN108530647A - The preparation method of organotitanium precursor body polymer TPP-I and its application in static conductive coating - Google Patents
The preparation method of organotitanium precursor body polymer TPP-I and its application in static conductive coating Download PDFInfo
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- 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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- 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
- C09D5/10—Anti-corrosive paints containing metal dust
- C09D5/106—Anti-corrosive paints containing metal dust containing Zn
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
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Abstract
The preparation method of organotitanium precursor body polymer TPP I and its application in static conductive coating, belong to preparation and the applied technical field of new material, by hydride powder, epoxy resin, nano-dispersing agent, titanate coupling agent, the mixture of silane coupling agent and solvent is placed in ball-milling reaction tank, ball-milling reaction is carried out under ultrasound condition, titanium valve is set to cause the chemical bond of polymer and the lattice key fracture of titanium nanoparticle surface during nanosizing, generate surface-active high ion or group, make polymer degradation at small molecule oligomer, graft polymerization reaction can occur at high temperature under high pressure, realize that molecular structure is reformed, obtain organotitanium precursor body polymer TPP I, it can be used for preparing the priming paint and finishing coat of static conductive coating.
Description
Technical field
The invention belongs to the preparation of new material and applied technical fields, and in particular to Mechano-chemical Synthesizing titanium nano-high molecule
The new process of alloy polymers and the manufacturing method of new material.
Background technology
It is well known that titanium is a kind of very active metallic element, density is small, and specific strength is high, and ductility is good, thermal coefficient
Low, resistant of high or low temperature is good, nontoxic nonmagnetic, wear resistant corrosion resistant, is widely used in the manufactures such as military project, space flight, navigation, civilian neck
Domain is known as space and the structural material of ocean.Titanium is arranged in Group IV subgroup (titanium family) element in the periodic table of chemical element
In system, atomic number 22, atomic weight 47.88, chemical valence has+2 ,+3 ,+4 three kinds.Therefore, it under certain environmental conditions, lives
Bold and vigorous property also provides the reaction tendency of diversity for it.
The standard electrode potential of titanium is very low (E=- 1.63V), causes blunt current potential also low, therefore is easy passivation.Under room temperature, titanium surface
The passivating film being made of oxide and nitride is easily formed, it is all highly stable in air and many erosion media, tool
There is good corrosion resistance.In air, aqueous chloride solution and oxidizing acid (nitric acid, chromic acid etc.) and most of organic acids,
Corrosion resistance has been more than stainless steel；It is not corroded substantially in the seawater, therefore is ocean
The optimal material of engineering.
Although Titanium has so good corrosion-resistance characteristics, titanium metal material is expensive, therefore to so far also
It cannot be prepared into erosion shield, lose field for industrial antisepsis.
If Titanium and high-molecular organic material " grafting " are formed high polymer alloy alloy state polymer, then with coating
Form promote the use of industrial antisepsis erosion field, not only alternative stainless steel, but also solve the problems, such as industrial corrosion, moreover it is possible to significantly
Manufacturing cost is reduced, improves the economic benefit of enterprise, here it is the purpose of the present invention and cause.
Organotitanium polymer (Organotitanium polymer), also known as poly- titanoxane (polytitanoxane) are
The general name of organometallic polymer containing titanium atom in backbone molecule structure, can be by orthotitanate Ti (OR)4It is partially hydrolysed
Aftercondensated forms.Poly- titanoxane can be used as surfactant, water repellent agent and antirust agent, can form fiber under mechanical stirring；Have
It can be used as preparing heat-resisting paint, this is example of the early stage using organic titanium manufacture coating.
Invention content
An object of the present disclosure is to prepare organotitanium precursor body polymer TPP-I.
The technical scheme is that：By hydride powder, epoxy resin, nano-dispersing agent, titanate coupling agent, silane coupled
The mixture of agent and solvent is placed in ball-milling reaction tank, and ball-milling reaction is carried out under ultrasound condition, among ball-milling reaction process
Discharge H with having a rest2, can opening feeding is to get organotitanium precursor body polymer after temperature in ball-milling reaction tank is cooled to 40~50 DEG C
TPP-I。
In mechanical milling process, TiH2H can be discharged2, therefore intermittent discharge H is carried out in the reaction2, then it is further continued for running.
Composition principle of the present invention：By the coupling of mechanical force and ultrasonic wave, not only it is refined to micron order titantium hydride
Nanoscale, while will also induce high molecular polymer and chain rupture graft polymerization reaction occurs, lead to epoxy resin and titanium atom knot
Symphysis is at the polymer (TPP-I) for retaining epoxy group.Its synthetic product reaction equation is：
The technology used in the present invention route is to be based on mechanical force and chemical principle, by Titanium and epoxy blend, by super
Sound wave auxiliary solid losses technology prepares nano-titanium base-material.According to《Mechanochemistry principle》（Chen Ding in 2008, old middle grey hair
Table in《Chemical Industry Press》Principle, polymer is under mechanical force, since internal stress is unevenly distributed or impact energy
Amount concentrates on individual segments, and generating limit stress makes chemical bond rupture.Most important feature is generationization when chemical bond rupture
Center (free radical).The position of power degradation (chemical bond rupture) depends on the stress concentrations on the individual segments of polymer, branched
Containing heteroatomic place and deformable polymer with horizontal key, the main chain at the node of main chain branch, in network in polymer
When stress concentration some node at.The present invention prepares nano organic titanium precursor polymer, and epoxy resin knot is exactly utilized
Containing this feature of hetero atom on structure main chain, chain rupture is occurred by the effect of mechanochemistry, and be bonded in titanium atom, formed a kind of
The metal-containing polymer of new results.
The present invention makes titanium valve draw during nanosizing using the activity of Titanium under the action of mechanical force and chemical
The chemical bond of polymer and the lattice key fracture of titanium nanoparticle surface are sent out, surface-active high ion or group is generated, makes
At small molecule oligomer graft polymerization reaction can occur at high temperature under high pressure for polymer degradation, realize that molecular structure is reformed, formed
A kind of precursor polymer of brand new.
Further, hydride powder of the present invention, epoxy resin, nano-dispersing agent, titanate coupling agent and silane are even
The mixing quality ratio for joining agent is 20~25: 15~20: 5~10: 1~3: 1~3.Hydride powder (TiH2) containing there are two hydrogen very
Two hydrogen atoms that are important, being capable of providing when graft polymerization reacts on titanium shoulder.And the hydride powder of not all addition can
Polymerisation is participated in, the titanium for not participating in reaction is filled in nano-hybrid particle in polymer, and carrying out enhancing to polymer changes
Property；Since nano-particle activity is high, easily reunite, therefore suitable nanometer hyper-dispersant is selected to be very important, selection principle
It is the small molecule type for being necessary for oligomer, i.e. its particle is less than titanium nano-particle, can just be coated on titanium nanoparticle surface shape
At corona layer, according to the principle that same electricity repels each other, the titanium nano-particle being wrapped by would not reunite, but uniformly and stably be divided
It dissipates in polymeric system；Coupling agent is also referred to as " bridging agent ", plays the compatibility effect of inorganic-organic phase.
The grain size of the hydride powder is 3~5 μm, belongs to fine titanium valve, can greatly shorten Ball-milling Time.But
Nanometer titanium power is directly bought, being such as without ball milling cannot be direct applied.Nanometer titanium power is only in the effect of mechanical force
Under, the epoxy polymer that could be deformed with disordering scission of link occurs molecule reformation and is graft-polymerized, and forms new polymer.
The nanometer hyper-dispersant is CI-913.
In ball-milling reaction, the volume ratio of ball material is about 6: 1, in ball-milling reaction tank the load volume amount of material be two/
One.
In ball-milling reaction, ball-milling reaction pressure inside the tank is 0.6MPa, temperature is 150 ± 1 DEG C.Pressure in ball grinder is come
Dehydrogenation reaction when from ball milling titanium valve and the hydrogen discharged.Temperature comes from the thermal accumlation in mechanical milling process, this is just machine
Tool chemical conversion provides energy source for thermochemical and creates condition.
The solvent is made of DMF, dimethylacetylamide (DMAC) and NMP mixing.DMF, DMAC and NMP, these solvents
All it is the carrier of solid losses, polymerisation carries out in the carrier.
The present invention another object is that propose using above method prepare organotitanium precursor body polymer TPP-I application,
It can be used for preparing the priming paint and finishing coat of static conductive coating.
When preparing static conductive coating bottom paint vehicle, by epoxy active diluent, organotitanium precursor body polymer TPP-I, ring
Then oxygen resin, LNBR, KH-560, GDS, mica powder and coating additive mixed grinding add super-fine zinc dust and carry out high speed point
After dissipating, using filter, static conductive coating priming paint is made.
When preparing static conductive coat side paint vehicle, by epoxy active diluent, organotitanium precursor body polymer TPP-I,
NPEL-128EP, YDJ-26LNBR, KH-560, colour carbon black, GDS, mica powder and coating additive mixed grinding, through filtering, system
Obtain static conductive tricoat finish.
When in use with priming material or finishing coat, it is used after scene is mixed with suitable curing agent, under the conditions of 25 DEG C,
It can reach surface drying in 2 hours, can reach within 24 hours and do solid work, can be realized within 5~7 days and drying is fully cured.Coating after drying, it is resistance to
Oiliness, salt fog resistance, oil resistivity are all fabulous, and surface resistivity is up to 106Ω has fabulous static conductive effect.
Description of the drawings
Fig. 1 is the titanium-based material electron microscopic picture before ball-milling reaction.
Fig. 2 is the electron microscopic picture after ball-milling reaction.
The scanning electron microscope that Fig. 3 is organotitanium precursor body polymer TPP-I characterizes picture.
Fig. 4 is the transmission electron microscope partial enlargement picture of organotitanium precursor body polymer TPP-I.
Specific implementation mode
One, planetary ultrasonic wave added solid-liquid ball-milling reaction device explanation：
Operation principle：When needing to apply the effect of ultrasonic wave, then the plug of supersonic generator is inserted into energy converter
On socket, the switch on supersonic generator is opened simultaneously, energy transfer machine is started to work at this time, and ultrasonic wave can input.By
In ultrasonic wave there is very strong penetration capacity, the stainless steel plate that energy penetration thickness is 2mm physics occurs to the material in ball grinder
Chemical action.
The technical parameter of ultrasonic wave added solid-liquid ball-milling reaction device is arranged：
(1) epicyclic transmission mechanism：18~168 r/min of autobiography (turntable), 70~670 r/min of revolution (ball grinder).
(2) ultrasonic frequency：40KHz.
(3) ultrasonic power：200 W.
(4) ultrasonic intensity：1.13 W/cm3。
Two, the preparation of organotitanium precursor body polymer TPP-I：
By the hydride powder (TiH of 20~25 mass parts2, 3~5 μm of grain size Φ, content >=99.5%, the Central-South limited public affairs of titanium valve high-tech
Department produce), 15~20 mass parts, 128 epoxy resin (Yueyang petrochemical industry product), 10~15 mass parts DMF, 8~12 mass parts diformazans
(C＆I is full of in German section for CI-913 nanometers of yl acetamide (DMAC), 15~20 mass parts NMP, 5~10 mass parts hyper-dispersants
CoeIen ChIme products), 1~3 mass parts titanate coupling agent and 1~3 mass parts silane coupling agent mixing.
Mixture uniformly mixed above is divided into quarter, is respectively charged into four ball-milling reaction tanks, each ball milling
Useful load in retort is half, then loads the stainless shot of four kinds of gradings respectively in each ball-milling reaction tank
(Φ 5, Φ 10, Φ 15, Φ 20mm) at 2/3rds, the volume ratio of ball material is about 6: 1, makes each ball milling anti-after fastening bolt
It answers tank to seal, opens ultrasonic wave and ball milling device.
In mechanical milling process, TiH2H can be discharged2, therefore shut down after running 1h, opening air bleeding valve is further continued for operation 2h and stops after deflating
Machine.During ball-milling reaction, it is about 150 DEG C that the pressure in ball grinder, which is controlled in 0.6MPa, temperature,.
Can opening feeding is to get poly- to black thick color liquid organotitanium precursor body when temperature in tank is cooled to 40~50 DEG C
It closes
Object TPP-I.
Each index parameter of organotitanium precursor body polymer TPP-I is listed in upper table.
Three, the characterization of each material：
From the electron microscopic picture before the ball-milling reaction of Fig. 1：By hydride powder, epoxy resin, nano-dispersing agent, titanate esters coupling
The titanium-based material of agent, silane coupling agent and solvent composition is a kind of mixing cluster states.
From electron microscopic picture after the ball-milling reaction of Fig. 2：Material complete nanosizing after solid-liquid ball-milling reaction.
Picture is characterized from the scanning electron microscope of the organotitanium precursor body polymer TPP-I of Fig. 3：The dispersion of nanosizing material
State.
From the transmission electron microscope partial enlargement picture of the organotitanium precursor body polymer TPP-I of Fig. 4：Solid-liquid ball-milling reaction
Core in object is titanium nano-particle, and shade covered section is polymer, and nucleocapsid constitutes titanium nanometer precursor polymer, as has
Machine titanium precursors polymer TPP-I.
Four, the preparation of petroleum storage tanks static conductive coating：
The coating is bi-component normal temperature cure self-drying type anti-corrosion function coating, divides priming paint and finishing coat, by A groups (paint vehicle) and B groups (Gu
Agent) packing.Specific preparation process is as follows：
1. priming paint：
5~10 parts of F-680 epoxy active diluents, 15~20 parts of TPP-I, 10~15 parts of NPEL-128 epoxies are weighed by mass parts
Resin (EP), 5~8 parts of LNBR, 0.5~1 part of KH-560,5~10 part of 6% graphene dispersion slurry (GDS), 3~5 part of 800 mesh mica
Powder, 3~5 parts of coating additives, are sequentially placed into high speed dispersor and are disperseed, and are ground to sand mill after being mixed and require fineness, so
After add 40~45 parts of super-fine zinc dust, high speed dispersion 20~30 minutes is divided after the assay was approved then with 200 mesh filter-cloth filterings
Dress, obtains priming paint A1.
2. the preparation of finishing coat
5~10 parts of F-680 epoxy active diluents, 15~20 parts of TPP-I, 30~35 parts of NPEL-128EP, 5 are weighed by mass parts
~10 parts of YDJ-26LNBR, 0.5~1 part of KH-560,3~5 parts of pigment charcoals, 5~10 part of 6% graphene dispersion slurry (GDS), 5~10
Part 800 mesh mica powders, 2~5 parts of coating additives put into container and are built in high speed dispersor and disperseed, used after being mixed successively
Sand mill is ground, and then with 200 mesh filter-cloth filterings, is dispensed after the assay was approved, as finishing coat A2.
3. curing agent is mating
TE-80A low viscosity epoxy curing agent is selected to do mating.
Mating application is as follows：
The mixing quality of priming paint and curing agent is：10∶1.
The mixing quality of finishing coat and curing agent is：4~5: 1.
The main component and quality of the above graphene dispersion slurry (GDS) contain admittedly is：Graphene (powder) 8%, nano-dispersing agent
8%, silane coupling agent 3%, 128 epoxy resin 20%, suspending agent 1%, surplus are the organic solvents such as N-Methyl pyrrolidone (NMP),
Mechanical dispersion is assisted using ultrasonic wave.
Five, the performance test results of oil tank static conductive functional anticorrosive paint：
It sees the above table.
Claims (9)
1. the preparation method of organotitanium precursor body polymer TPP-I, by hydride powder, epoxy resin, nanometer hyper-dispersant, metatitanic acid
The mixture of ester coupling agent, silane coupling agent and solvent is placed in ball-milling reaction tank, and it is small that ball-milling reaction 3 is carried out under ultrasound condition
When, intermittently discharge H during ball-milling reaction2, the can opening feeding after temperature in ball-milling reaction tank is cooled to 40~50 DEG C, i.e.,
Obtain organotitanium precursor body polymer TPP-I.
2. the preparation method of organotitanium precursor body polymer TPP-I according to claim 1, it is characterised in that the titantium hydride
Powder, epoxy resin, nano-dispersing agent, titanate coupling agent and silane coupling agent mixing quality ratio be 20~25: 15~20: 5
~10: 1~3: 1~3.
3. the preparation method of organotitanium precursor body polymer TPP-I according to claim 1 or claim 2, it is characterised in that the hydrogen
The grain size for changing titanium valve is 3~5 μm.
4. the preparation method of organotitanium precursor body polymer TPP-I according to claim 1 or claim 2, it is characterised in that described to receive
Rice hyper-dispersant is CI-913.
5. the preparation method of organotitanium precursor body polymer TPP-I according to claim 1 or claim 2, it is characterised in that in ball milling
When reaction, the volume ratio of ball material is about 6: 1, and the load volume amount of material is half in ball-milling reaction tank.
6. the preparation method of organotitanium precursor body polymer TPP-I according to claim 1 or claim 2, it is characterised in that it is described
When ball-milling reaction, ball-milling reaction pressure inside the tank is 0.6MPa, temperature is 150 ± 1 DEG C.
7. the preparation method of organotitanium precursor body polymer TPP-I according to claim 1 or claim 2, it is characterised in that described molten
Agent is made of DMF, dimethylacetylamide and NMP mixing.
8. organotitanium precursor body polymer TPP-I prepared by method as described in claim 1 is used to prepare in static conductive coating bottom
Paint vehicle, it is characterised in that by epoxy active diluent, organotitanium precursor body polymer TPP-I, epoxy resin, LNBR, KH-560,
GDS, mica powder and coating additive mixed grinding, using filter, are made and lead after then adding super-fine zinc dust progress high speed dispersion
Electrostatic coating priming paint material.
9. organotitanium precursor body polymer TPP-I prepared by method as described in claim 1 is used to prepare in static conductive coat side
Paint vehicle, it is characterised in that by epoxy active diluent, organotitanium precursor body polymer TPP-I, NPEL-128EP, YDJ-
Static conductive tricoat finish is made through filtering in 26LNBR, KH-560, pigment charcoal, GDS, mica powder and coating additive mixed grinding
Material.
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| CN111548705A (en) * | 2020-06-05 | 2020-08-18 | 哈尔滨鑫科纳米科技发展有限公司 | Titanium nano polymer resin and preparation method and application thereof |
| CN111635657A (en) * | 2020-05-11 | 2020-09-08 | 兰州星河石化防腐有限公司 | Titanium-based polymer alloy welding seam protection coating functional material and preparation method thereof |
| CN112390956A (en) * | 2021-01-19 | 2021-02-23 | 泽铱(佛山)工业技术有限公司 | Hydroxyl organic titanium polymer and preparation method and application thereof |
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Application publication date: 20180914 |