CN108503841A - The preparation method of organotitanium precursor body polymer TPP-II and its application in sapecial coating - Google Patents
The preparation method of organotitanium precursor body polymer TPP-II and its application in sapecial coating Download PDFInfo
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- C09D185/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon; Coating compositions based on derivatives of such polymers
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- 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
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Abstract
The preparation method of organotitanium precursor body polymer TPP II and its application in sapecial coating, belong to preparation and the applied technical field of new material.γUnder the catalysis of phase nano aluminium oxide, 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, pass through the coupling of mechanical force and ultrasonic wave, micron order titantium hydride is not only set to be refined to nanoscale, high molecular polymer will be also induced simultaneously, and chain rupture graft polymerization reaction occurs, then open loop generates the organotitanium precursor body polymer TPP II of hydroxyl structure to epoxy group, it can be used for preparing hot environment acid resistance corrosion protection coating, such as flue gas desulphurization system and the priming paint and finishing coat of heat exchange equipment.
Description
Technical field
The invention belongs to the preparation of new material and applied technical fields.
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 the optimal material of ocean engineering.
Although Titanium has so good corrosion-resistance characteristics, titanium metal material is expensive, can't incite somebody to action so far
It is prepared into erosion shield, loses field for industrial antisepsis.
If Titanium and high-molecular organic material " grafting " are formed high polymer alloy state polymer, then with the shape of coating
Formula promotes the use of industrial antisepsis erosion field, not only alternative stainless steel, but also solves the problems, such as industrial corrosion, moreover it is possible to substantially reduce
Manufacturing cost improves the economic benefit of enterprise, and 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
First purpose of the invention is to prepare a kind of organotitanium precursor body polymer TPP-II.
The technical scheme is that：γUnder the catalysis of phase nano aluminium oxide, by hydride powder, epoxy resin, nanometer point
Powder, titanate coupling agent, silane coupling agent and solvent mixture be placed in ball-milling reaction tank, ball is carried out under ultrasound condition
Mill reaction, H is intermittently discharged during ball-milling reaction2, can opening takes after temperature is cooled to 40~50 DEG C in ball-milling reaction tank
Material is to get organotitanium precursor body polymer TPP-II.
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：In catalystγ-Phase nano aluminium oxide (γ-Al2O3-x ) under effect, by mechanical force with
The coupling of ultrasonic wave not only makes micron order titantium hydride be refined to nanoscale, while will also induce high molecular polymer hair
Raw chain rupture graft polymerization reaction, then open loop generates the phenoxy polymer (TPP-II) of hydroxyl structure to epoxy group；It synthesizes production
Object 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.
This reaction is divided into two processes：First stage is that metallic titanium powder titanium nano-particle interface during nanosizing is former
Son absorbs energy and discharges H2Process；Second stage isγPhase nano aluminium oxide (γ-Al2O3-x ) vacant key (oxygen debt key) with
Epoxy group fights for oxygen atom, and give off energy (exothermic process), forces epoxy ring-opening, so as to cause the fracture of C-O carbon-oxygen bonds
And be bonded with titanium atom, form nano organic titanium precursor polymer.
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, the polymer are a kind of universal titanium-based material, can be used alone the base for doing coating
Body material can also be blended with various kinds of resin (such as EP, PY, PET, PI, EP-PF, PAES, PAEK), and it is multiple to prepare high polymer alloy
It is used further to production coating after closing object or copolymer.
Further, of the present inventionγPhase nano aluminium oxide, hydride powder, epoxy resin, nanometer hyper-dispersant, titanium
The mixing quality of acid esters coupling agent and silane coupling agent ratio is 1~5: 20~25: 15~20: 5~10: 1~3: 1~3.Titantium hydride
Powder (TiH2) hydrogen is extremely important containing there are two, two hydrogen atoms being capable of providing when graft polymerization reacts on titanium shoulder.Not
The hydride powder of all additions can participate in polymerisation, do not participate in the titanium of reaction and be filled in polymer with nano-hybrid particle and work as
In, enhancing modification is carried out to polymer；Since nano-particle activity is high, easily reunites, therefore select suitable nanometer hyper-dispersant
It is very important, selection principle is the small molecule type for being necessary for oligomer, i.e. its particle is less than titanium nano-particle, could wrap
It is overlying on titanium nanoparticle surface and forms corona layer, according to the principle that same electricity repels each other, the titanium nano-particle being wrapped by would not reunite
, but be uniformly and stably scattered in polymeric system；Coupling agent is also referred to as " bridging agent ", plays the phase of inorganic-organic phase
Appearance acts on.
The grain size of the hydride powder is 3~5 μm, belongs to fine titanium valve, can greatly shorten Ball-milling Time.And it is direct
Nanometer titanium power is bought, being without ball milling cannot be direct applied.Nanometer titanium power is only under the action of mechanical force,
The epoxy polymer that can be deformed with disordering scission of link occurs molecule and reforms and be graft-polymerized, and forms new polymer.
It is describedγGrain size≤20 μm of phase nano aluminium oxide.Use the grain sizeγPhase nano aluminium oxide makees catalyst,
It easily causes polymer molecule and chemical bond rupture occurs, form active centre.
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-II application,
It can be used for preparing hot environment acid resistance corrosion protection coating, such as flue gas desulphurization system and the priming paint and finishing coat of heat exchange equipment.
When being used to prepare flue gas desulphurization system and heat exchange equipment priming paint, by carbonate mixed ester, propene carbonate, organic titanium
Precursor polymer TPP-II, epoxy resin, NPCN-704PFEP, Desmophen 670SP, carbon black, graphene dispersion slurry, cloud
Female powder, rust resisting pigment, curing agent, diaminodiphenylsulfone, R-8747MEA and coating additive are ground after mixing, through filtering, system
Obtain priming paint material.
When being used to prepare flue gas desulphurization system and heat exchange equipment finishing coat, by carbonate mixed ester, propene carbonate, organic titanium
Precursor polymer TPP-II, epoxy resin, NPCN-704PFEP, Desmophen 670SP, carbon black, graphene dispersion slurry, cloud
Female powder, rust resisting pigment, diaminodiphenylsulfone and R-8747MEA and coating additive are ground after mixing, and through filtering, finishing coat is made
Material.
Before brushing, first equipment metal surface is handled, after exposing steel material, then carries out priming paint successively
With the brushing of finishing coat, reapplied after dry solidification in equipment operation.Through experiment, desulfurization has been fully met to coat
Heat-resisting, wear-resisting, resistant to chemical media the requirement of system equipment operation.
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-II characterizes picture.
Fig. 4 is the transmission electron microscope partial enlargement picture of organotitanium precursor body polymer TPP-II.
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)；Revolve round the sun 70~670 r/min (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-II：
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), 1~5 mass parts VK-L20YγPhase nano aluminium oxide (γ-Al2O3-x , grain size≤20 μm, Xuancheng
The production and sales of Jing Rui new materials Co., Ltd), 1~3 mass parts titanate coupling agent, 1~3 mass parts silane coupling agent mixing it is equal
It is even.
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 to black thick color liquid organotitanium precursor body when temperature in tank is cooled to 40~50 DEG C
Polymer TPP-II.
Each index parameter is listed in upper table.
Three, the characterization of each material：
From the electron microscopic picture before the ball-milling reaction of Fig. 1：ByγPhase nano aluminium oxide, hydride powder, epoxy resin, nanometer
The titanium-based material that dispersant, titanate coupling agent, silane coupling agent and solvent form 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-II of Fig. 3：Point of nanosizing material
Bulk state.
From the transmission electron microscope partial enlargement picture of the organotitanium precursor body polymer TPP-II of Fig. 4：Solid-liquid ball milling is anti-
It is titanium nano-particle to answer the core in object, and shade covered section is polymer, and nucleocapsid constitutes titanium nanometer precursor polymer, as
Organotitanium precursor body polymer TPP-II.
Four, flue gas desulphurization system and heat exchange equipment coating are made：
1. priming paint：
Priming paint component A：In terms of mass parts, 5~10 parts of carbonate mixed esters (DXC or HEMA), 2~8 parts of propene carbonates are weighed
(PDC), 10~15 parts of TPP-II, 5~10 part of 609 (E-03) epoxy resin (EP), 5~10 parts of NPCN-704PFEP, 3~6 parts
Desmophen 670SP, 3~5 parts of MA-100 Mitsubishi Carbon Blacks, 5~10 part of 6% graphene dispersion slurry (GDS), 5~10 part of 800 mesh
Mica powder, 15~20 parts of TFG-1 Composite Anticorrosive Pigment Usings, 20~25 part of ten thousand China's TH-100 HDI trimers, 3~5 parts of diamino two
Benzene sulfone (DDS), 3~5 parts of R-8747MEA and 3~5 part of coating additive input containers are built in high speed dispersor and are disperseed, and mix
It uses sand mill to grind afterwards, is then packed with 200 mesh filter-cloth filterings.
Priming paint B component：20~25 parts of TH-100 HDI trimers curing agent, can direct packaging.
In use, after mixing by priming paint component A and the scenes priming paint B, being painted on the flue gas desulfurization device of surface cleaning
Or heat exchanger metal material surface forms prime coat after 25 DEG C dry.
2. finishing coat：
Finishing coat component A：In terms of mass parts, 5~10 parts of carbonate mixed esters (DXC or HEMA), 2~8 parts of propene carbonates are weighed
(PDC), 10~15 parts of TPP-II, 5 ~ 10 part of 609 (E-03) epoxy resin (EP), 5~10 parts of NPCN-704PFEP, 3~6 parts
Desmophen 670SP, 3~5 parts of MA-100 Mitsubishi Carbon Blacks, 5~10 part of 6% graphene dispersion slurry (GDS), 5~10 part of 800 mesh
Mica powder, 15~20 parts of TFG-1 Composite Anticorrosive Pigment Usings, 3~5 parts of diaminodiphenylsulfones (DDS), 3~5 parts of R-8747MEA and 3~
5 parts of coating additive input containers, which are built in high speed dispersor, to be disperseed, and is ground using sand mill after being mixed, then with 200 mesh
Filter-cloth filtering is packed.
Finishing coat B component：20~25 parts of TH-100 HDI trimer curing agent, direct packaging.
In use, after mixing by finishing coat component A and the scenes finishing coat B, cured primer coat surface is painted on, through 25 DEG C
After drying, topcoat is formed.
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.
The performance test results of flue gas desulphurization system and heat exchange equipment coating are seen the above table.
Claims (10)
1. the preparation method of organotitanium precursor body polymer TPP-II, it is characterised in that：γThe catalysis of phase nano aluminium oxide
Under, the mixture of hydride powder, epoxy resin, nanometer hyper-dispersant, titanate coupling agent, silane coupling agent and solvent is placed in
In ball-milling reaction tank, ball-milling reaction is carried out under ultrasound condition 3 hours, H is intermittently discharged during ball-milling reaction2, wait for ball
Can opening feeding is to get organotitanium precursor body polymer TPP-II after temperature is cooled to 40~50 DEG C in mill retort.
2. the preparation method of organotitanium precursor body polymer TPP-II according to claim 1, it is characterised in that describedγPhase
The mixing quality ratio of nano aluminium oxide, hydride powder, epoxy resin, nano-dispersing agent, titanate coupling agent and silane coupling agent
It is 1~5: 20~25: 15~20: 5~10: 1~3: 1~3.
3. the preparation method of organotitanium precursor body polymer TPP-II 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-II according to claim 1 or claim 2, it is characterised in that describedγGrain size≤20 μm of phase nano aluminium oxide.
5. the preparation method of organotitanium precursor body polymer TPP-II according to claim 1 or claim 2, it is characterised in that described to receive
Rice hyper-dispersant is CI-913.
6. the preparation method of organotitanium precursor body polymer TPP-II 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.
7. the preparation method of organotitanium precursor body polymer TPP-II according to claim 1 or claim 2, it is characterised in that in ball milling
When reaction, ball-milling reaction pressure inside the tank is 0.6MPa, temperature is 150 ± 1 DEG C.
8. the preparation method of organotitanium precursor body polymer TPP-II according to claim 1 or claim 2, it is characterised in that described molten
Agent is made of DMF, dimethylacetylamide (DMAC) and NMP mixing.
9. organotitanium precursor body polymer TPP-II prepared by method as described in claim 1 be used to prepare flue gas desulfurization device and
The priming paint of heat exchanger, it is characterised in that by carbonate mixed ester, propene carbonate, organotitanium precursor body polymer TPP-II, epoxy
Resin, NPCN-704PFEP, Desmophen 670SP, carbon black, graphene dispersion slurry, mica powder, rust resisting pigment, curing agent, two
Aminodiphenyl sulfone, R-8747MEA and coating additive are ground after mixing, and through filtering, priming paint material is made.
10. organotitanium precursor body polymer TPP-II prepared by method as described in claim 1 is used to prepare flue gas desulfurization device
And the finishing coat of heat exchanger, it is characterised in that by carbonate mixed ester, propene carbonate, organotitanium precursor body polymer TPP-II, ring
Oxygen resin, NPCN-704PFEP, Desmophen 670SP, carbon black, graphene dispersion slurry, mica powder, rust resisting pigment, diamino
Diphenyl sulphone (DPS) and R-8747MEA and coating additive are ground after mixing, and through filtering, finishing coat material is made.
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| PCT/CN2018/086003 WO2019210528A1 (en) | 2018-05-02 | 2018-05-08 | Preparation method for organic titanium precursor polymer tpp-ii and application thereof in special coating |
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| CN111607324A (en) * | 2020-05-18 | 2020-09-01 | 广东健玺表面工程技术有限公司 | Super-hydrophobic anti-drag anticorrosive coating for inner coating of oil and gas pipeline and preparation method thereof |
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| CN112390958A (en) * | 2021-01-19 | 2021-02-23 | 泽铱(佛山)工业技术有限公司 | Titanium-based polymer alloy copolymer and preparation method and application thereof |
| CN112391115A (en) * | 2021-01-19 | 2021-02-23 | 泽铱(佛山)工业技术有限公司 | Special coating for titanium-based polymer alloy oil well pipe and preparation method thereof |
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