CN108239473A - A kind of preparation method of lower shrinkage ultraviolet-curing paint - Google Patents

A kind of preparation method of lower shrinkage ultraviolet-curing paint Download PDF

Info

Publication number
CN108239473A
CN108239473A CN201711488483.4A CN201711488483A CN108239473A CN 108239473 A CN108239473 A CN 108239473A CN 201711488483 A CN201711488483 A CN 201711488483A CN 108239473 A CN108239473 A CN 108239473A
Authority
CN
China
Prior art keywords
parts
ultraviolet
necked flask
preparation
curing
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201711488483.4A
Other languages
Chinese (zh)
Inventor
谭春容
何少雄
陈可
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Changzhou Huambo Metal Component Factory
Original Assignee
Changzhou Huambo Metal Component Factory
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Changzhou Huambo Metal Component Factory filed Critical Changzhou Huambo Metal Component Factory
Priority to CN201711488483.4A priority Critical patent/CN108239473A/en
Publication of CN108239473A publication Critical patent/CN108239473A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D175/00Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
    • C09D175/04Polyurethanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F257/00Macromolecular compounds obtained by polymerising monomers on to polymers of aromatic monomers as defined in group C08F12/00
    • C08F257/02Macromolecular compounds obtained by polymerising monomers on to polymers of aromatic monomers as defined in group C08F12/00 on to polymers of styrene or alkyl-substituted styrenes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F263/00Macromolecular compounds obtained by polymerising monomers on to polymers of esters of unsaturated alcohols with saturated acids as defined in group C08F18/00
    • C08F263/02Macromolecular compounds obtained by polymerising monomers on to polymers of esters of unsaturated alcohols with saturated acids as defined in group C08F18/00 on to polymers of vinyl esters with monocarboxylic acids
    • C08F263/04Macromolecular compounds obtained by polymerising monomers on to polymers of esters of unsaturated alcohols with saturated acids as defined in group C08F18/00 on to polymers of vinyl esters with monocarboxylic acids on to polymers of vinyl acetate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F290/00Macromolecular compounds obtained by polymerising monomers on to polymers modified by introduction of aliphatic unsaturated end or side groups
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40High-molecular-weight compounds
    • C08G18/63Block or graft polymers obtained by polymerising compounds having carbon-to-carbon double bonds on to polymers
    • C08G18/635Block or graft polymers obtained by polymerising compounds having carbon-to-carbon double bonds on to polymers onto unsaturated polymers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72Polyisocyanates or polyisothiocyanates
    • C08G18/74Polyisocyanates or polyisothiocyanates cyclic
    • C08G18/76Polyisocyanates or polyisothiocyanates cyclic aromatic
    • C08G18/7614Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/14Polycondensates modified by chemical after-treatment
    • C08G59/1433Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds
    • C08G59/1438Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds containing oxygen
    • C08G59/1455Monocarboxylic acids, anhydrides, halides, or low-molecular-weight esters thereof
    • C08G59/1461Unsaturated monoacids
    • C08G59/1466Acrylic or methacrylic acids
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2227Oxides; Hydroxides of metals of aluminium
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Wood Science & Technology (AREA)
  • Materials Engineering (AREA)
  • Engineering & Computer Science (AREA)
  • Emergency Medicine (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Macromonomer-Based Addition Polymer (AREA)
  • Paints Or Removers (AREA)

Abstract

The invention discloses a kind of preparation methods of lower shrinkage ultraviolet-curing paint, belong to technical field of paint preparation.When carrying out carbonation decomposition to sodium aluminate solution with carbon dioxide in the present invention and preparing aluminium hydroxide powder, the Crater corrosion of sodium aluminate solution reduces, in ultraviolet-curing paint, aluminum hydroxide particles are better to the gapfill of modified epoxy acrylate resin particle, ultraviolet-curing paint is in the curing process in the present invention, part aluminum hydroxide particles can react generation nano silicon dioxide with sodium metasilicate in dispersion glue, nanometer silicon dioxide particle is coated on resin particle surfaces, improve the curing efficiency of coating, the low shrinkage additive that polystyrene similar in cure shrinkage is major ingredient is used for modified epoxy acrylate resin, steric hindrance increases during cure shrinkage, reticular structure makes paint film have certain tensile property, so as to reduce the cure shrinkage of ultraviolet-curing paint, increase the flexibility of paint film, it has a extensive future.

Description

A kind of preparation method of lower shrinkage ultraviolet-curing paint
Technical field
The invention discloses a kind of preparation methods of lower shrinkage ultraviolet-curing paint, belong to technical field of paint preparation.
Background technology
Ultraviolet-curing paint is that light-initiated there is chemically active liquid material quickly to be polymerize, hand over using ultraviolet Connection etc. reactions and rapid curing film forming a kind of coating.It is a kind of the coating material solidified of high-efficiency environment friendly, has curing rate soon, admittedly Change temperature it is low, production efficiency is high, save the energy, without organic solvent, be suitble to flow line production the advantages that.It is organic molten due to being free of Agent, so as to eliminate pollution of the volatile organic compounds to environment significantly.First part of patent of ultraviolet-curing paint is born Nineteen forty-seven, by the development of over half a century, UV is coating material solidified to have become more mature technology, in particular with people's ring The raising of consciousness is protected, production and researcher are important to note that the coating material solidified development and application of UV.UV coating material solidified is a kind of green Color environment-friendly type coating, it complies fully with " 4E " principle, and general UV curings energy consumption is the 1/5 of heat cure, and UV is coating material solidified containing waving It is less to send out component, pollution is small, most attract researcher and developer to be that UV is coating material solidified can reduce raw materials consumption, be conducive to Reduce financial cost.
Corrosion of metal is the phenomenon that metal is destroyed by chemistry or the electrochemical action of surrounding medium, is passed through to its people Ji brings huge loss.Metal equipment anticorrosion is most effective, one of most common method is exactly anti-in metal surface coating Corrosion resistant coating, to completely cut off contact of the corrosive medium with metallic matrix, predominantly hot-melt asphalt adds winding glass wool cloth, epoxy resin Coating, scale resin coating, inorganic zinc coating etc..
With the fast development of world economy and the continuous improvement of people's quality of the life, environmental protection and energy saving more next It is more taken seriously, the coating that Speeding up development uses no or little organic solvent namely develops " Environmentally friendly coatings " and become generation The common recognition of various countries of boundary.Environmentally friendly coatings mainly have powdery paints, radiation curable coating etc..
At present, widely applied UV curable ink is mainly free radical type ink in print field, is had fast The advantages that fast curing, high glaze, good weatherability, but due to polymer volume contraction in radical polymerization process, make ink Flexibility is poor.
Therefore, invent a kind of lower shrinkage ultraviolet-curing paint has positive effect to technical field of paint preparation.
Invention content
Present invention mainly solves the technical issues of, for ultraviolet-curing paint curing when shrinking percentage it is big, can cause to paint The defects of film flexibility is poor provides a kind of preparation method of lower shrinkage ultraviolet-curing paint.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is:
A kind of preparation method of lower shrinkage ultraviolet-curing paint, it is characterised in that specifically preparation process is:
(1)The sodium aluminate solution that 700~800mL mass fractions are 20% is put into plastic channel, with the rate of 20~30mL/min Lead to 40~45min of carbon dioxide gas into plastic channel, after ventilation, 3~4h of standing sedimentation obtains sedimentation mixture, will Sedimentation mixture is placed in horizontal table filter, and filtering removal filtrate obtains filter residue, and filter residue is placed in baking oven, is heated to 90 ~100 DEG C, dry 4~5h obtains aluminium hydroxide powder;
(2)Aluminium hydroxide powder is placed in high pressure draught machine, 10~15min of air-flow crushing, it is 50~80 μm to obtain grain size 200~220g aluminium hydroxide superfine powders are poured into the sodium metasilicate equipped with 500~550mL mass fractions 30% by aluminium hydroxide superfine powder In solution, colloidal fluid is obtained, colloidal fluid is placed in high speed dispersor and is obtained with the rotating speed high speed dispersion of 3000~3300r/min Disperse glue;
(3)It counts in parts by weight, 60~70 parts of polystyrene and 30~40 parts of vinyl acetate resins is mixed, obtain compound tree Hybrid resin is poured into the three-necked flask equipped with 60~70 parts of styrene, 80~90 DEG C is heated to three-necked flask by fat, Start blender, be dispersed with stirring with the rotating speed of 300~350r/min, insulated and stirred reacts 4~5h, and discharging is naturally cooling to room Temperature obtains low shrinkage additive;
(4)50~60gE-51 epoxy resin and 4~5g triethanolamines are added in three-necked flask, oil bath heating is warming up to 70~ 80 DEG C, start blender, start to stir with the rotating speed of 300~350r/min, with dropping funel to four-hole boiling flask with 2~3mL/ 40~50mL acrylic acid is added dropwise into three-necked flask for the drop rate of min, reacts 2~3h, obtains epoxy acrylic resin;
(5)Continue to add in 10~15mL trimethylolpropane allyl ethers into three-necked flask, be warming up to 90~95 DEG C, heat preservation React 1~2h, add 8~10 parts of toluene di-isocyanate(TDI)s, after being cooled to 110~120 DEG C, into four-hole boiling flask add in 20~ 30 parts of propylene glycol monomethyl ethers are diluted, and continue to be cooled to 80 DEG C, add in triethylamine and distilled water adjusts reaction solution in three-necked flask PH is 8.0~8.5, discharges after 20~25min of stirring and obtains modified epoxy acrylate resin;
(6)Count in parts by weight, weigh 70~80 parts of modified epoxy acrylate resins, 5~10 parts dispersion glues, 8~12 parts it is different Phorone, 10~15 parts of low shrinkage additives are put into high speed dispersor, with the rotating speed high speed dispersion 15 of 2000~3000r/min After~18min, lower shrinkage ultraviolet-curing paint is obtained.
The beneficial effects of the invention are as follows:
(1)The present invention is passed through carbon dioxide into sodium aluminate solution, and standing sedimentation obtains sedimentation mixture, filtered, dry To aluminium hydroxide powder, aluminium hydroxide powder and sodium silicate solution high speed dispersion are obtained uniformly disperseing glue, by polyphenyl second Alkene is poured into after being mixed with vinyl acetate resin in styrene, and low shrinkage additive is obtained by the reaction in insulated and stirred, by E-51 asphalt mixtures modified by epoxy resin Acrylic acid is added dropwise after being mixed with triethanolamine in fat, and epoxy acrylic resin is obtained by the reaction, three are added in into epoxy acrylic resin Hydroxymethyl-propane diallyl ether, continuously adds toluene di-isocyanate(TDI) after reaction, it is dilute to add propylene glycol monomethyl ether for insulation reaction It releases, adjusts reaction product pH and obtain modified epoxy acrylate resin, finally by modified epoxy acrylate resin, dispersion glue, low The high speed dispersions such as shrink additives obtain lower shrinkage ultraviolet-curing paint, in the present invention with carbon dioxide to sodium aluminate solution into When row carbonation decomposition prepares aluminium hydroxide powder, the Crater corrosion of sodium aluminate solution reduces, and decomposing crystal seed of aluminum hydroxide is pressed down System, the hydroxide particle-size that surrounding is formed attenuate, and in ultraviolet-curing paint, aluminium hydroxide is discontinuous phase, and resin particle is Continuous phase, aluminum hydroxide particles granularity is smaller, and specific surface area is bigger, bigger with resin particle contact area in coating, hydroxide Alumina particles are better to the gapfill of modified epoxy acrylate resin particle, and shrinking percentage reduces during so as to make paint solidification;
(2)Ultraviolet-curing paint in the curing process, disperses part aluminum hydroxide particles meeting and silicic acid in glue in the present invention Sodium reaction generation nano silicon dioxide, nanometer silicon dioxide particle is coated on resin particle surfaces, affine to the moisture in coating Degree is high, can accelerate water content of coating and be migrated into paint film, improve the curing efficiency of coating, make for modified epoxy acrylate resin The polystyrene similar in cure shrinkage is the low shrinkage additive of major ingredient, this kind of low shrinkage additive is a kind of core shell structure Material, inner core be styrene, can be combined in the curing process with epoxy group, form the tridimensional network of diverging, Gu Change steric hindrance when shrinking to increase, reticular structure makes paint film have certain tensile property, so as to make ultraviolet-curing paint Cure shrinkage reduces, and increases the flexibility of paint film, has a extensive future.
Specific embodiment
The sodium aluminate solution that 700~800mL mass fractions are 20% is put into plastic channel, with the speed of 20~30mL/min Rate leads to 40~45min of carbon dioxide gas into plastic channel, and after ventilation, 3~4h of standing sedimentation obtains sedimentation mixture, Sedimentation mixture is placed in horizontal table filter, filtering removal filtrate obtains filter residue, and filter residue is placed in baking oven, is heated to 90~100 DEG C, dry 4~5h obtains aluminium hydroxide powder;Aluminium hydroxide powder is placed in high pressure draught machine, air-flow crushing 10~15min obtains the aluminium hydroxide superfine powder that grain size is 50~80 μm, 200~220g aluminium hydroxide superfine powders is poured into dress In the sodium silicate solution for having 500~550mL mass fractions 30%, obtain colloidal fluid, by colloidal fluid be placed in high speed dispersor with The rotating speed high speed dispersion of 3000~3300r/min obtains dispersion glue;It counts in parts by weight, by 60~70 parts of polystyrene and 30 ~40 parts of vinyl acetate resin mixing, obtain hybrid resin, and hybrid resin is poured into three mouthfuls of burnings equipped with 60~70 parts of styrene In bottle, 80~90 DEG C are heated to three-necked flask, starts blender, is dispersed with stirring with the rotating speed of 300~350r/min, is protected Temperature is stirred to react 4~5h, and discharging is naturally cooling to room temperature and obtains low shrinkage additive;By 50~60gE-51 epoxy resin and 4 ~5g triethanolamines are added in three-necked flask, and oil bath heating is warming up to 70~80 DEG C, start blender, with 300~350r/min Rotating speed start to stir, be added dropwise into three-necked flask to four-hole boiling flask 40 with the drop rate of 2~3mL/min with dropping funel~ 50mL acrylic acid reacts 2~3h, obtains epoxy acrylic resin;Continue to add in 10~15mL trihydroxy methyls into three-necked flask Propane diallyl ether is warming up to 90~95 DEG C, 1~2h of insulation reaction, adds 8~10 parts of toluene di-isocyanate(TDI)s, cooling To after 110~120 DEG C, into three-necked flask, 20~30 parts of propylene glycol monomethyl ethers of addition are diluted, and are continued to be cooled to 80 DEG C, be added in It is 8.0~8.5 that triethylamine and distilled water, which adjust reaction solution pH in four-hole boiling flask, discharges after 20~25min of stirring and obtains modified ring Oxypropylene acid resin;Count in parts by weight, weigh 70~80 parts of modified epoxy acrylate resins, 5~10 parts dispersion glues, 8~ 12 parts of isophorones, 10~15 parts of low shrinkage additives are put into high speed dispersor, with the rotating speed of 2000~3000r/min at a high speed After disperseing 15~18min, lower shrinkage ultraviolet-curing paint is obtained.
Example 1
The sodium aluminate solution that 700mL mass fractions are 20% is put into plastic channel, is led to the rate of 20mL/min into plastic channel Carbon dioxide gas 40min, after ventilation, standing sedimentation 3h obtains sedimentation mixture, and sedimentation mixture is placed on square position mistake In filter, filtering removal filtrate obtains filter residue, and filter residue is placed in baking oven, is heated to 90 DEG C, and dry 4h obtains hydroxide Aluminium powder material;Aluminium hydroxide powder is placed in high pressure draught machine, air-flow crushing 10min, obtains the aluminium hydroxide that grain size is 50 μm 200g aluminium hydroxide superfine powders are poured into the sodium silicate solution equipped with 500mL mass fractions 30%, obtain colloidal fluid by superfine powder, Colloidal fluid is placed in high speed dispersor, dispersion glue is obtained with the rotating speed high speed dispersion of 3000r/min;It counts in parts by weight, it will 60 parts of polystyrene and 30 parts of vinyl acetate resin mixing, obtain hybrid resin, hybrid resin are poured into equipped with 60 parts of styrene Three-necked flask in, be heated to 80 DEG C to three-necked flask, start blender, be dispersed with stirring with the rotating speed of 300r/min, protect Temperature is stirred to react 4h, and discharging is naturally cooling to room temperature and obtains low shrinkage additive;By tri- ethyl alcohol of 50gE-51 epoxy resin and 4g Amine is added in three-necked flask, and oil bath heating is warming up to 70 DEG C, is started blender, is started to stir with the rotating speed of 300r/min, with drop 40mL acrylic acid is added dropwise into three-necked flask with the drop rate of 2mL/min to four-hole boiling flask for liquid funnel, reacts 2h, obtains epoxy Acroleic acid resin;Continue to add in 10mL trimethylolpropane allyl ethers into three-necked flask, be warming up to 90 DEG C, insulation reaction 1h adds 8 parts of toluene di-isocyanate(TDI)s, and after being cooled to 110 DEG C, it is dilute that 20 parts of propylene glycol monomethyl ethers progress are added in into three-necked flask It releases, continues to be cooled to 80 DEG C, it is 8.0 to add in reaction solution pH in triethylamine and distilled water adjusting four-hole boiling flask, is gone out after stirring 20min Material obtains modified epoxy acrylate resin;Count in parts by weight, weigh 70 parts of modified epoxy acrylate resins, 5 parts dispersion glues, 8 parts of isophorones, 10 parts of low shrinkage additives are put into high speed dispersor, with the rotating speed high speed dispersion 15min of 2000r/min Afterwards, lower shrinkage ultraviolet-curing paint is obtained.
Example 2
The sodium aluminate solution that 750mL mass fractions are 20% is put into plastic channel, is led to the rate of 25mL/min into plastic channel Carbon dioxide gas 42min, after ventilation, standing sedimentation 3.5h obtains sedimentation mixture, and sedimentation mixture is placed on square position In filter, filtering removal filtrate obtains filter residue, and filter residue is placed in baking oven, is heated to 95 DEG C, and dry 4.5h obtains hydrogen Alumina powder;Aluminium hydroxide powder is placed in high pressure draught machine, air-flow crushing 12min, obtains the hydrogen-oxygen that grain size is 70 μm Change aluminium superfine powder, 210g aluminium hydroxide superfine powders are poured into the sodium silicate solution equipped with 525mL mass fractions 30%, obtain glue Colloidal fluid is placed in high speed dispersor and obtains dispersion glue with the rotating speed high speed dispersion of 3150r/min by shape liquid;In parts by weight 65 parts of polystyrene and 35 parts of vinyl acetate resins are mixed, obtain hybrid resin, hybrid resin is poured into equipped with 65 parts of benzene by meter In the three-necked flask of ethylene, 85 DEG C are heated to three-necked flask, starts blender, with the rotating speed stirring point of 320r/min It dissipates, insulated and stirred reaction 4.5h, discharging is naturally cooling to room temperature and obtains low shrinkage additive;By 55gE-51 epoxy resin and 4g Triethanolamine is added in three-necked flask, and oil bath heating is warming up to 75 DEG C, is started blender, is started to stir with the rotating speed of 320r/min It mixes, 45mL acrylic acid is added dropwise into three-necked flask with the drop rate of 2mL/min to four-hole boiling flask with dropping funel, react 2.5h obtains epoxy acrylic resin;Continue to add in 12mL trimethylolpropane allyl ethers into three-necked flask, be warming up to 92 DEG C, insulation reaction 1.5h, 9 parts of toluene di-isocyanate(TDI)s are added, after being cooled to 115 DEG C, 25 parts are added in into three-necked flask Propylene glycol monomethyl ether is diluted, and continues to be cooled to 80 DEG C, is added in reaction solution pH in triethylamine and distilled water adjusting four-hole boiling flask and is Discharging obtains modified epoxy acrylate resin after 8.2, stirring 22min;It counts in parts by weight, weighs 75 parts of modified epoxy acrylic acid Resin, 7 parts of dispersion glues, 10 parts of isophorones, 12 parts of low shrinkage additives are put into high speed dispersor, with 2500r/min's After rotating speed high speed dispersion 16min, lower shrinkage ultraviolet-curing paint is obtained.
Example 3
The sodium aluminate solution that 800mL mass fractions are 20% is put into plastic channel, is led to the rate of 30mL/min into plastic channel Carbon dioxide gas 45min, after ventilation, standing sedimentation 4h obtains sedimentation mixture, and sedimentation mixture is placed on square position mistake In filter, filtering removal filtrate obtains filter residue, and filter residue is placed in baking oven, is heated to 100 DEG C, and dry 5h obtains hydrogen-oxygen Change aluminium powder material;Aluminium hydroxide powder is placed in high pressure draught machine, air-flow crushing 15min, obtains the hydroxide that grain size is 80 μm 220g aluminium hydroxide superfine powders are poured into the sodium silicate solution equipped with 550mL mass fractions 30%, obtain glue by aluminium superfine powder Colloidal fluid is placed in high speed dispersor and obtains dispersion glue with the rotating speed high speed dispersion of 3300r/min by liquid;In parts by weight 70 parts of polystyrene and 40 parts of vinyl acetate resins are mixed, obtain hybrid resin, hybrid resin is poured into equipped with 70 parts of benzene by meter In the three-necked flask of ethylene, 90 DEG C are heated to three-necked flask, starts blender, with the rotating speed stirring point of 350r/min It dissipates, insulated and stirred reaction 5h, discharging is naturally cooling to room temperature and obtains low shrinkage additive;By 60 gE-51 epoxy resin and 5g Triethanolamine is added in three-necked flask, and oil bath heating is warming up to 80 DEG C, is started blender, is started to stir with the rotating speed of 350r/min It mixes, 50mL acrylic acid is added dropwise into three-necked flask with the drop rate of 3mL/min to four-hole boiling flask with dropping funel, reacts 3h, Obtain epoxy acrylic resin;Continue to add in 15mL trimethylolpropane allyl ethers into three-necked flask, be warming up to 95 DEG C, Insulation reaction 2h adds 10 parts of toluene di-isocyanate(TDI)s, and after being cooled to 120 DEG C, 30 parts of propylene glycol are added in into three-necked flask Methyl ether is diluted, and continues to be cooled to 80 DEG C, and it is 8.5 to add in reaction solution pH in triethylamine and distilled water adjusting four-hole boiling flask, is stirred Discharging obtains modified epoxy acrylate resin after mixing 25min;Count in parts by weight, weigh 80 parts of modified epoxy acrylate resins, 10 parts of dispersion glues, 12 parts of isophorones, 15 parts of low shrinkage additives are put into high speed dispersor, with the rotating speed of 3000r/min After high speed dispersion 18min, lower shrinkage ultraviolet-curing paint is obtained.
Comparative example
It is ultraviolet to lower shrinkage produced by the present invention as a comparison case with the lower shrinkage ultraviolet-curing paint that Suzhou company produces Lower shrinkage ultraviolet-curing paint in photocureable coating and comparative example carries out performance detection, and testing result is as shown in table 1:
1st, test method:
Flexibility test is detected with flexibility tester, observes coating embrittlement situation;
Hardness test is represented using pencil hardness;
Table 1
Test event Example 1 Example 2 Example 3 Comparative example
Flexibility Not embrittlement Not embrittlement Not embrittlement Embrittlement
Hardness(H) 4H 4H 4H 2H
Adhesive force(Grade) 0 1 1 4
Tensile strength(MPa) 40 41 42 31
The flexibility of lower shrinkage ultraviolet-curing paint produced by the present invention is good according to above-mentioned middle data, and tensile strength is high, So as to reduce the cure shrinkage of ultraviolet-curing paint, the flexibility for increasing paint film has broad application prospects.

Claims (7)

1. a kind of preparation method of lower shrinkage ultraviolet-curing paint, it is characterised in that specifically preparation process is:
(1)700~800mL sodium aluminate solutions are put into plastic channel, carbon dioxide gas is led into plastic channel, ventilation finishes Afterwards, standing sedimentation obtains sedimentation mixture, and sedimentation mixture is placed in horizontal table filter, and filtering removal filtrate obtains filter residue, Filter residue is placed in baking oven, heat temperature raising, it is dry, obtain aluminium hydroxide powder;
(2)Aluminium hydroxide powder is placed in high pressure draught machine, air-flow crushing, obtains aluminium hydroxide superfine powder, by 200~220g Aluminium hydroxide superfine powder is poured into equipped in 500~550mL sodium silicate solutions, obtains colloidal fluid, and colloidal fluid is placed in high speed dispersion Machine middling speed disperses to obtain dispersion glue;
(3)It counts in parts by weight, 60~70 parts of polystyrene and 30~40 parts of vinyl acetate resins is mixed, obtain compound tree Fat pours into hybrid resin in the three-necked flask equipped with 60~70 parts of styrene, to three-necked flask heat temperature raising, starts blender It is dispersed with stirring, insulated and stirred reaction, discharging is naturally cooling to room temperature and obtains low shrinkage additive;
(4)50~60 gE-51 epoxy resin and 4~5g triethanolamines are added in three-necked flask, oil bath heating heating starts Blender starts to stir, and 40~50mL acrylic acid is added dropwise into three-necked flask to four-hole boiling flask with dropping funel, ring is obtained by the reaction Oxypropylene acid resin;
(5)Continue to add in 10~15mL trimethylolpropane allyl ethers into three-necked flask, heating, insulation reaction, then add Enter 8~10 parts of toluene di-isocyanate(TDI)s, cool down, 20~30 parts of propylene glycol monomethyl ethers are added in into four-hole boiling flask and are diluted, are continued Cooling, adds in triethylamine and distilled water adjusts reaction solution pH in three-necked flask, and discharging after stirring obtains modified epoxy acrylic acid tree Fat;
(6)Count in parts by weight, weigh 70~80 parts of modified epoxy acrylate resins, 5~10 parts dispersion glues, 8~12 parts it is different After phorone, 10~15 parts of low shrinkage additives are put into the dispersion of high speed dispersor high speed, obtain the curing of lower shrinkage ultraviolet light and apply Material.
2. a kind of preparation method of lower shrinkage ultraviolet-curing paint according to claim 1, it is characterised in that:Step (1)The mass fraction of the sodium aluminate solution is 20%, and Ventilation Rate is 20~30mL/min, duration of ventilation for 40~ 45min, standing sedimentation time are 3~4h, and temperature is 90~100 DEG C after heat temperature raising, and drying time is 4~5h.
3. a kind of preparation method of lower shrinkage ultraviolet-curing paint according to claim 1, it is characterised in that:Step (2)The air-flow crushing time is 10~15min, and the grain size of aluminium hydroxide superfine powder is 50~80 μm, sodium silicate solution Mass fraction is 30%, and high speed dispersor rotating speed is 3000~3300r/min.
4. a kind of preparation method of lower shrinkage ultraviolet-curing paint according to claim 1, it is characterised in that:Step (3)Described is 80~90 DEG C to temperature after three-necked flask heat temperature raising, and speed of agitator is 300~350r/min, insulated and stirred Reaction time is 4~5h.
5. a kind of preparation method of lower shrinkage ultraviolet-curing paint according to claim 1, it is characterised in that:Step (4)Temperature is 70~80 DEG C after described oil bath heating heating, and speed of agitator is 300~350r/min, drop rate for 2~ 3mL/min, reaction time are 2~3h.
6. a kind of preparation method of lower shrinkage ultraviolet-curing paint according to claim 1, it is characterised in that:Step (5)Temperature is 90~95 DEG C after the heating, and the insulation reaction time is 1~2h, and temperature is 110~120 DEG C after cooling, is continued Temperature is 80 DEG C after cooling, and it is 8.0~8.5 to add in reaction solution pH in triethylamine and distilled water adjusting three-necked flask, mixing time For 20~25min.
7. a kind of preparation method of lower shrinkage ultraviolet-curing paint according to claim 1, it is characterised in that:Step (6)The high speed dispersor rotating speed is 2000~3000r/min, and the high speed dispersion time is 15~18min.
CN201711488483.4A 2017-12-30 2017-12-30 A kind of preparation method of lower shrinkage ultraviolet-curing paint Pending CN108239473A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201711488483.4A CN108239473A (en) 2017-12-30 2017-12-30 A kind of preparation method of lower shrinkage ultraviolet-curing paint

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201711488483.4A CN108239473A (en) 2017-12-30 2017-12-30 A kind of preparation method of lower shrinkage ultraviolet-curing paint

Publications (1)

Publication Number Publication Date
CN108239473A true CN108239473A (en) 2018-07-03

Family

ID=62701268

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201711488483.4A Pending CN108239473A (en) 2017-12-30 2017-12-30 A kind of preparation method of lower shrinkage ultraviolet-curing paint

Country Status (1)

Country Link
CN (1) CN108239473A (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110016278A (en) * 2019-03-06 2019-07-16 常州市三伊化工有限公司 A kind of preparation method of the anti-scratch black finish of dumb light
CN110305519A (en) * 2019-06-12 2019-10-08 王银梅 A kind of preparation method of high grade of transparency flatting silica
CN110396867A (en) * 2019-06-12 2019-11-01 刘雄 A kind of preparation method of food packaging leaching membrane paper
CN114574075A (en) * 2022-04-12 2022-06-03 江苏中基复合材料有限公司 Aluminum foil for resin-coated aluminum foil cover plate and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104910757A (en) * 2015-05-11 2015-09-16 广德美涂士化工有限公司 Heat-resistant ultraviolet curing coating
CN107022283A (en) * 2017-03-28 2017-08-08 常州大学 A kind of preparation method of ultraviolet light curing cathodic electrophoretic coating compound resin

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104910757A (en) * 2015-05-11 2015-09-16 广德美涂士化工有限公司 Heat-resistant ultraviolet curing coating
CN107022283A (en) * 2017-03-28 2017-08-08 常州大学 A kind of preparation method of ultraviolet light curing cathodic electrophoretic coating compound resin

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110016278A (en) * 2019-03-06 2019-07-16 常州市三伊化工有限公司 A kind of preparation method of the anti-scratch black finish of dumb light
CN110305519A (en) * 2019-06-12 2019-10-08 王银梅 A kind of preparation method of high grade of transparency flatting silica
CN110396867A (en) * 2019-06-12 2019-11-01 刘雄 A kind of preparation method of food packaging leaching membrane paper
CN114574075A (en) * 2022-04-12 2022-06-03 江苏中基复合材料有限公司 Aluminum foil for resin-coated aluminum foil cover plate and preparation method thereof
CN114574075B (en) * 2022-04-12 2023-01-20 江苏中基复合材料有限公司 Aluminum foil for resin-coated aluminum foil cover plate and preparation method thereof

Similar Documents

Publication Publication Date Title
CN108239473A (en) A kind of preparation method of lower shrinkage ultraviolet-curing paint
CN106221666B (en) A kind of high thermal conductivity, high-adhesive-strength organosilicon casting glue and preparation method thereof and its method for encapsulating motor end
CN101892004B (en) Ultraviolet-cured heat-resistant coating and preparation and application methods thereof
CN103319916B (en) Preparation method of inorganic-organic double-layer coated type aluminum paste
CN101407651A (en) UV curing color decorative coating
CN105176287A (en) Heat-resistant and flame-retardant modified acrylic emulsion paint
CN102304319A (en) Preparation method of H-grade water-solubility silicon steel sheet paint
CN104559419A (en) Thermal-insulating powder coating and preparation method thereof
CN108084803A (en) A kind of preparation method of silane-modified carbon black color paste
CN101235232B (en) Nano silicon dioxide modifying water composite road sign dope and preparation method thereof
CN106833247A (en) A kind of environment-friendly type fluorine carbon anticorrosive paint and preparation method thereof
CN110358395A (en) A kind of corrosion-resistant finishes and preparation method thereof based on graphene
CN102585648B (en) Laser electrolytic aluminum film regeneration coating and preparation method thereof
CN109868015A (en) A kind of organo-mineral complexing is aluminum paint, aqueous and preparation method thereof
CN104650697A (en) High temperature resistant nano coating
CN111117555A (en) Environment-friendly aqueous adhesive and preparation method thereof
CN106675152A (en) Extinction modifier for powder coating, application of extinction modifier and extinction powder coating containing extinction modifier
CN109880496A (en) A kind of bumper quick-dry type coating and preparation method thereof
CN105925058B (en) A kind of preparation method of the UV luminous printing ink of resistance to plateau climate
CN103013203A (en) Compound type ultraviolet light-cured anticorrosive paint and preparation method thereof
CN102977666B (en) Zirconia loaded metal antirust paint and its preparation method
CN108219622A (en) It is a kind of based on the aluminium alloy of graphene low-density anticorrosive paint and preparation method thereof
CN104327667B (en) A kind of preparation method for dry and wet transformator solvent-free Self-leveling iron core coating varnish
CN105348958B (en) A kind of water-based dumb light coating varnish of two-component organic inorganic hybridization and preparation method thereof and construction method
CN110408295A (en) A kind of preparation method of acidproof waterproof corrosion-resistant epoxy paint

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20180703

RJ01 Rejection of invention patent application after publication