CN110093080A - A kind of preparation method of anti-oxidant aqueous automobile paint - Google Patents

A kind of preparation method of anti-oxidant aqueous automobile paint Download PDF

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CN110093080A
CN110093080A CN201910206066.9A CN201910206066A CN110093080A CN 110093080 A CN110093080 A CN 110093080A CN 201910206066 A CN201910206066 A CN 201910206066A CN 110093080 A CN110093080 A CN 110093080A
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parts
automobile paint
temperature
aqueous automobile
desciccate
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谭祖生
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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
    • C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
    • C09D133/04—Homopolymers or copolymers of esters
    • C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • C09D133/10—Homopolymers or copolymers of methacrylic acid esters
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/63—Additives non-macromolecular organic
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/65—Additives macromolecular
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2217—Oxides; Hydroxides of metals of magnesium
    • C08K2003/222—Magnesia, i.e. magnesium oxide
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
    • C08L2205/16—Fibres; Fibrils

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Paints Or Removers (AREA)

Abstract

The present invention relates to a kind of preparation methods of anti-oxidant aqueous automobile paint, belong to technical field of paint preparation.Reacting slurry is made using bagasse and taro skin as raw material in the present invention, and reacting slurry is concentrated and dried to grind, grinding product is made, finally by grinding product and water, resin solvent and the mixing of other auxiliary agents discharge up to anti-oxidant aqueous automobile paint, sugar is isolated in present invention extraction, the substances such as plant fiber, generation carboxyl is decomposed simultaneously, epoxy group, hydroxyl, furfural etc., to improve the bonding degree in aqueous automobile paint between each molecule and the bonding adsorption strength with substrate surface, present invention introduces aluminium ions and magnesium ion, metal ion and fiber and sugared part molecule are adsorbed by chelation and ionic bond and other Chemical bondings, coating is set to have the protection of compact metal oxide protective film on surface layer, make coating that there is good inoxidizability and mechanical strength, it has a good application prospect.

Description

A kind of preparation method of anti-oxidant aqueous automobile paint
Technical field
The present invention relates to a kind of preparation methods of anti-oxidant aqueous automobile paint, belong to technical field of paint preparation.
Background technique
With the rapid development of social economy with the raising of living standards of the people, the automobile production sales volume in China rapidly sent out Exhibition.Automobile is chronically exposed to open air, is often subject to the erosion of the adverse circumstances factors such as rainwater, dust, high temperature solarization, oxidation.
Car paint just refers to the coating being painted on the various types of vehicles such as car vehicle body and components, refers generally to the painting of new car Material and auxiliary material and vehicle repairing coating.Car paint is generally made of film forming matter (resin), auxiliary agent, pigment, solvent. Car paint is sprayed on automobile, vehicle body can be made to be not easy to be corroded.Car paint should generally have the advantage that (1) The appearance for beautifying vehicle, makes automobile appearance seem more pleasing, gives aesthetic feeling；(2) fabulous mechanical performance adapts to vapour The high speed of vehicle, more shake and strain, it is desirable that the adhesive force of paint film is good, hard flexible, impact resistance, resist bending, damage resistant, rub resistance etc. Superior performance；(3) fabulous scrub resistance, resistance to soiling and it is good can toolability；(4) fabulous weatherability and corrosion resistance, Can be suitably used for various temperature, exposure and erosion by wind and rain, keep in a variety of weather conditions not loss of gloss, it is non-discolouring, do not crack, do not take off It falls.
Currently, car paint used in most domestic bus, bus factory belongs to solvent-based paints, containing a large amount of harmful Material composition does not meet environmentally protective requirement.In recent years, since people are to the pay attention to day by day of environment, volatile organic matter Discharge is just limited by being increasingly stringenter.Water paint is to take water as a solvent to be prepared, and is easy to get with raw material, technique letter Single, at low cost, easy for construction, easily stored, stable mechanical performance, form a film smooth, water resistance and excellent corrosion resistance etc. Feature.But since the surface tension of water is larger, evaporation rate is slow, makes water paint in coating process to the warm, wet of environment Degree variation is more sensitive, is easy to produce the various paint film defects such as bubble, cissing, sagging, and dirt easy to attach, high-temperature resistant result Bad, antioxidant effect is bad, in addition, there is also the defects of wear-resisting property difference.
Therefore, it is necessary to develop the aqueous automobile paint that a kind of high-temperature resistant result is good, antioxidant effect is good to have important meaning Justice.
Summary of the invention
The technical problems to be solved by the invention: easily rupturable for current aqueous automobile paint, fall off, antioxygenic property is poor Defect, provide a kind of preparation method of anti-oxidant aqueous automobile paint.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
The specific preparation step of anti-oxidant aqueous automobile paint are as follows:
It weighs grinding product, aqueous methacrylic acid ethyl ester resin, deionized water, isocyanates, zinc chromate, triethanolamine and gathers Amide is put into reaction kettle, is increased temperature in the kettle to 65~75 DEG C, is mixed under conditions of revolving speed is 200~240r/min 80~100min discharges up to anti-oxidant aqueous automobile paint；
The specific preparation step of grinding product are as follows:
(1) desciccate, aluminium chloride, magnesium chloride, citric acid, propanedione and dehydrated alcohol are put into three-necked flask, with stirring 3~4h is mixed with the revolving speed of 500~600r/min in device, and it is 12~16% that mass fraction is added dropwise after stirring into three-necked flask Sodium hydroxide solution adjust pH value to 11~12 obtained reaction mixtures；
(2) oxidizing gas is passed through with the rate of 120~140mL/min into reaction mixture, is continually fed into 65~75min, Three-necked flask is placed in sonic oscillation instrument after being passed through, 3~4h is vibrated under conditions of frequency is 32~36kHz, it will after oscillation Three-necked flask is placed in resistance heating set, increases jacket temperature to 110~120 DEG C, 55~65min of heated at constant temperature, is made anti- Answer slurries；
The specific preparation step of desciccate is
(1) by bagasse and taro skin investment baking oven, dry 3~4h, throws after dry under conditions of temperature is 65~75 DEG C Entering in planetary ball mill, 60~80min of mixed grinding is made grounds travel and minces under conditions of revolving speed is 200~260r/min, Grounds travel is minced and is put into beaker with mass fraction for 8~12% hydrochloric acid, with blender with the revolving speed of 400~500r/min 2~3h is mixed, mixed solution is made；
(2) mixed solution is put into reaction kettle, nitrogen is filled with into reaction kettle, until in kettle air pressure be increased to 1.3~ 1.5MPa seals reaction kettle, increases temperature in the kettle to 160~180 DEG C, constant temperature and pressure reacts 2~3h and reaction solution is made, and will react Liquid investment is concentrated and dried in device, and 2~3h is concentrated and dried under conditions of vacuum degree is 100~120Pa, temperature is 55~65 DEG C Desciccate is made.
According to parts by weight, the grinding product is 16~18 parts, aqueous methacrylic acid ethyl ester resin is 20~22 Part, deionized water are 26~30 parts, isocyanates is 2~3 parts, zinc chromate is 0.6~0.8 part, triethanolamine is 1~2 part, poly- Amide is 3~5 parts.
In the specific preparation step (1) of grinding product preferably according to parts by weight, desciccate is 6~8 parts, aluminium chloride For 0.4~0.8 part, magnesium chloride be 0.2~0.4 part, citric acid is 2~4 parts, propanedione is 5~7 parts, dehydrated alcohol be 13~ 15 parts.
It a small amount of hydrochloric acid can further be added dropwise in three-necked flask in the specific preparation step (1) of grinding product is mixed into and stir It mixes.
In the specific preparation step (2) of grinding product oxidizing gas be more preferably ozone, chlorine, nitric oxide its One of or a variety of mix in any proportion.
The mass ratio of bagasse and taro skin is 3:1 in the specific preparation step (1) of desciccate.
In the specific preparation step (1) of desciccate grounds travel mince with mass fraction be 8~12% hydrochloric acid mass ratio For 1:10.
Reaction kettle warming temperature is further preferably 172~176 DEG C in the specific preparation step (2) of desciccate.
The method have the benefit that:
(1) bagasse and taro skin are dried ground and mixed first by the present invention, are put into hydrochloric acid and are impregnated after grinding, high temperature after immersion Reaction under high pressure, dry obtained desciccate, desciccate is then mixed, pH value is adjusted after mixing with aluminium salt, magnesium salts after reaction To alkalinity, and it is passed through ozone gas reaction, is heated after reaction and reacting slurry is made, and reacting slurry is concentrated and dried grinding and is made Grinding product finally discharges grinding product and water, resin solvent and the mixing of other auxiliary agents up to anti-oxidant aqueous vapour Bagasse and taro skin after drying grinding, salt acid soak, high-temperature high-voltage reaction, are therefrom extracted and are divided by vehicle coating, the present invention Separate out the substances such as sugar molecule, plant fiber, at the same high-temperature high-voltage reaction make macromolecular fibre Surface Creation carboxyl, epoxy group, Substances such as hydroxyl, furfural, and macromolecular sugar part molecule decomposes fracture and generates the shorter polysaccharide molecule of chain length, sugared part molecule and have Machine fiber molecule improved in aqueous automobile paint by covalent bond, hydrogen bond and the absorption of other Chemical bondings each molecule it Between bonding degree and bonding adsorption strength with substrate surface, be difficult to rupture, scratch and fall off after making paint solidification, have Good mechanical strength；
(2) present invention introduces aluminium ion and magnesium ion, by reacting with lye and ozone, metal oxide, while gold are generated Belong to ion and fiber and sugared part molecule is adsorbed by chelation and ionic bond and the effect of other Chemical bondings, is conducive to In fibre composition surface, the metal oxide generated after making is grown in fiber surface, metal oxide benefit metal ion deposition It is more good to be bonded in coating with the good absorption property in a large amount of free external boundary of group contained in fibre composition, And be scattered in coating, aluminium oxide structure is fine and close, fine and close metal oxide protective film can be formed on coating surface layer, to coating It plays a good protective effect, makes coating that there is good inoxidizability, the nanoscale magnesium filled in coating can add The mechanical property of strong coating, enhances the impact resistance of coating and compressive property, has a good application prospect.
Specific embodiment
Bagasse and taro skin 3:1 in mass ratio are put into baking oven, dry 3 under conditions of temperature is 65~75 DEG C~ 4h is put into planetary ball mill after dry, and 60~80min of mixed grinding is made under conditions of revolving speed is 200~260r/min Grounds travel minces, and grounds travel is minced and is put into beaker with mass fraction for 8~12% hydrochloric acid 1:10 in mass ratio, with stirring Device is mixed 2~3h with the revolving speed of 400~500r/min and mixed solution is made；Above-mentioned mixed solution is put into reaction kettle, It is filled with nitrogen into reaction kettle, until air pressure is increased to 1.3~1.5MPa in kettle, seals reaction kettle, increases temperature in the kettle to 160 ~180 DEG C, constant temperature and pressure reacts 2~3h and reaction solution is made, and reaction solution is put into and is concentrated and dried in device, is 100 in vacuum degree ~120Pa, temperature are concentrated and dried 2~3h under conditions of being 55~65 DEG C and desciccate are made；According to parts by weight, by 6~8 parts Above-mentioned desciccate, 0.4~0.8 part of aluminium chloride, 0.2~0.4 part of magnesium chloride, 2~4 parts of citric acids, 5~7 parts of propanedione and 13 In~15 parts of dehydrated alcohol investment three-necked flasks, 3~4h, stirring are mixed with the revolving speed of 500~600r/min with blender The sodium hydroxide solution that mass fraction is 12~16% is added dropwise in backward three-necked flask and adjusts pH value to 11~12 obtained reaction mixing Liquid；Oxidizing gas is passed through with 120~140mL/min rate into above-mentioned reaction mixture, is continually fed into 65~75min, is led to Three-necked flask is placed in sonic oscillation instrument after entering, 3~4h is vibrated under conditions of frequency is 32~36kHz, by three after oscillation Mouth flask is placed in resistance heating set, increases jacket temperature to 110~120 DEG C, 55~65min of heated at constant temperature, reaction is made Slurries；Above-mentioned slurries are put into beaker, are placed the beaker in vacuum oven, vacuum degree is 120~140Pa, temperature is It is constant that it is concentrated in vacuo to product quality under conditions of 65~75 DEG C, obtains thickened solid, thickened solid is put into planetary ball mill In, 150~170min is ground under conditions of revolving speed is 300~360r/min, and grinding product is made；According to parts by weight, claim Take above-mentioned 16~18 parts of grinding products, 20~22 parts of aqueous methacrylic acid ethyl ester resins, 26~30 parts of deionized waters, 2~3 parts In isocyanates, 0.6~0.8 part of zinc chromate, 1~2 part of triethanolamine and 3~5 parts of polyamide investment reaction kettles, temperature in kettle is increased 80~100min is mixed to 65~75 DEG C in degree under conditions of revolving speed is 200~240r/min, discharges up to anti-oxidant water Property car paint.
Example 1
Oxidizing gas: ozone
The preparation of mixed solution:
By in bagasse and taro skin 3:1 in mass ratio investment baking oven, dry 3h, throws after dry under conditions of temperature is 65 DEG C Enter in planetary ball mill, mixed grinding 60min is made grounds travel and minces under conditions of revolving speed is 200r/min, will grind The hydrochloric acid 1:10 in mass ratio that object and mass fraction are 8% is put into beaker, is mixed with blender with the revolving speed of 400r/min Mixed solution is made in 2h.
The preparation of desciccate:
Above-mentioned mixed solution is put into reaction kettle, nitrogen is filled with into reaction kettle, until air pressure is increased to 1.3MPa in kettle, it is close Reaction kettle is sealed, increases temperature in the kettle to 160 DEG C, constant temperature and pressure reacts 2h and reaction solution is made, and reaction solution is put into and is concentrated and dried dress In setting, 2h is concentrated and dried under conditions of vacuum degree is 100Pa, temperature is 55 DEG C, desciccate is made.
The preparation of reaction mixture:
According to parts by weight, by 6 parts of above-mentioned desciccates, 0.4 part of aluminium chloride, 0.2 part of magnesium chloride, 2 parts of citric acids, 5 parts the third two In ketone and 13 parts of dehydrated alcohol investment three-necked flasks, 3h is mixed with the revolving speed of 500r/min with blender, to three after stirring The sodium hydroxide solution that mass fraction is 12% is added dropwise in mouth flask and adjusts pH value to 11 obtained reaction mixtures.
The preparation of reacting slurry:
Oxidizing gas is passed through with 120mL/min rate into above-mentioned reaction mixture, is continually fed into 65min, by three after being passed through Mouth flask is placed in sonic oscillation instrument, vibrates 3h under conditions of frequency is 32kHz, three-necked flask is placed in resistance after oscillation and is added In hot jacket, jacket temperature is increased to 110 DEG C, heated at constant temperature 55min, reacting slurry is made.
The preparation of grinding product:
Above-mentioned slurries are put into beaker, are placed the beaker in vacuum oven, vacuum degree is 120Pa, temperature is 65 DEG C Under the conditions of to be concentrated in vacuo to product quality constant, obtain thickened solid, thickened solid put into planetary ball mill, is in revolving speed 150min is ground under conditions of 300r/min, and grinding product is made.
The preparation of anti-oxidant aqueous automobile paint:
According to parts by weight, above-mentioned 16 parts of grinding products, 20 parts of aqueous methacrylic acid ethyl ester resins, 26 parts of deionizations are weighed In water, 2 parts of isocyanates, 0.6 part of zinc chromate, 1 part of triethanolamine and 3 parts of polyamide investment reaction kettles, temperature in the kettle is increased extremely 65 DEG C, 80min is mixed under conditions of revolving speed is 200r/min, discharges up to anti-oxidant aqueous automobile paint.
Example 2
Oxidizing gas: chlorine
The preparation of mixed solution:
By in bagasse and taro skin 3:1 in mass ratio investment baking oven, dry 3h, throws after dry under conditions of temperature is 70 DEG C Enter in planetary ball mill, mixed grinding 70min is made grounds travel and minces under conditions of revolving speed is 230r/min, will grind The hydrochloric acid 1:10 in mass ratio that object and mass fraction are 10% is put into beaker, is stirred with blender with the revolving speed mixing of 450r/min It mixes 2h and mixed solution is made.
The preparation of desciccate:
Above-mentioned mixed solution is put into reaction kettle, nitrogen is filled with into reaction kettle, until air pressure is increased to 1.4MPa in kettle, it is close Reaction kettle is sealed, increases temperature in the kettle to 170 DEG C, constant temperature and pressure reacts 2h and reaction solution is made, and reaction solution is put into and is concentrated and dried dress In setting, 2h is concentrated and dried under conditions of vacuum degree is 110Pa, temperature is 60 DEG C, desciccate is made.
The preparation of reaction mixture:
According to parts by weight, by 7 parts of above-mentioned desciccates, 0.6 part of aluminium chloride, 0.3 part of magnesium chloride, 3 parts of citric acids, 6 parts the third two In ketone and 14 parts of dehydrated alcohol investment three-necked flasks, 3h is mixed with the revolving speed of 550r/min with blender, to three after stirring The sodium hydroxide solution that mass fraction is 14% is added dropwise in mouth flask and adjusts pH value to 11 obtained reaction mixtures.
The preparation of reacting slurry:
Oxidizing gas is passed through with 130mL/min rate into above-mentioned reaction mixture, is continually fed into 70min, by three after being passed through Mouth flask is placed in sonic oscillation instrument, vibrates 3h under conditions of frequency is 34kHz, three-necked flask is placed in resistance after oscillation and is added In hot jacket, jacket temperature is increased to 115 DEG C, heated at constant temperature 60min, reacting slurry is made.
The preparation of grinding product:
Above-mentioned slurries are put into beaker, are placed the beaker in vacuum oven, vacuum degree is 130Pa, temperature is 70 DEG C Under the conditions of to be concentrated in vacuo to product quality constant, obtain thickened solid, thickened solid put into planetary ball mill, is in revolving speed 160min is ground under conditions of 330r/min, and grinding product is made.
The preparation of anti-oxidant aqueous automobile paint:
According to parts by weight, above-mentioned 17 parts of grinding products, 21 parts of aqueous methacrylic acid ethyl ester resins, 28 parts of deionizations are weighed In water, 2 parts of isocyanates, 0.7 part of zinc chromate, 1 part of triethanolamine and 4 parts of polyamide investment reaction kettles, temperature in the kettle is increased extremely 70 DEG C, 90min is mixed under conditions of revolving speed is 220r/min, discharges up to anti-oxidant aqueous automobile paint.
Example 3
Oxidizing gas: nitric oxide
The preparation of mixed solution:
By in bagasse and taro skin 3:1 in mass ratio investment baking oven, dry 4h, throws after dry under conditions of temperature is 75 DEG C Enter in planetary ball mill, mixed grinding 80min is made grounds travel and minces under conditions of revolving speed is 260r/min, will grind The hydrochloric acid 1:10 in mass ratio that object and mass fraction are 12% is put into beaker, is stirred with blender with the revolving speed mixing of 500r/min It mixes 3h and mixed solution is made.
The preparation of desciccate:
Above-mentioned mixed solution is put into reaction kettle, nitrogen is filled with into reaction kettle, until air pressure is increased to 1.5MPa in kettle, it is close Reaction kettle is sealed, increases temperature in the kettle to 180 DEG C, constant temperature and pressure reacts 3h and reaction solution is made, and reaction solution is put into and is concentrated and dried dress In setting, 3h is concentrated and dried under conditions of vacuum degree is 120Pa, temperature is 65 DEG C, desciccate is made.
The preparation of reaction mixture:
According to parts by weight, by 8 parts of above-mentioned desciccates, 0.8 part of aluminium chloride, 0.4 part of magnesium chloride, 4 parts of citric acids, 7 parts the third two In ketone and 15 parts of dehydrated alcohol investment three-necked flasks, 4h is mixed with the revolving speed of 600r/min with blender, to three after stirring The sodium hydroxide solution that mass fraction is 16% is added dropwise in mouth flask and adjusts pH value to 12 obtained reaction mixtures.
The preparation of reacting slurry:
Oxidizing gas is passed through with 140mL/min rate into above-mentioned reaction mixture, is continually fed into 75min, by three after being passed through Mouth flask is placed in sonic oscillation instrument, vibrates 4h under conditions of frequency is 36kHz, three-necked flask is placed in resistance after oscillation and is added In hot jacket, jacket temperature is increased to 120 DEG C, heated at constant temperature 65min, reacting slurry is made.
The preparation of grinding product:
Above-mentioned slurries are put into beaker, are placed the beaker in vacuum oven, vacuum degree is 140Pa, temperature is 75 DEG C Under the conditions of to be concentrated in vacuo to product quality constant, obtain thickened solid, thickened solid put into planetary ball mill, is in revolving speed 170min is ground under conditions of 360r/min, and grinding product is made.
The preparation of anti-oxidant aqueous automobile paint:
According to parts by weight, above-mentioned 18 parts of grinding products, 22 parts of aqueous methacrylic acid ethyl ester resins, 30 parts of deionizations are weighed In water, 3 parts of isocyanates, 0.8 part of zinc chromate, 2 parts of triethanolamines and 5 parts of polyamide investment reaction kettles, temperature in the kettle is increased extremely 75 DEG C, 100min is mixed under conditions of revolving speed is 240r/min, discharges up to anti-oxidant aqueous automobile paint.
Comparative example 1: it is essentially identical with the preparation method of embodiment 1, it has only the difference is that desciccate is not added.
Comparative example 2: it is essentially identical with the preparation method of embodiment 2, it has only the difference is that reaction mixture is not added.
Comparative example 3: the car paint of company, Shenzhen production.
Car paint in anti-oxidant aqueous automobile paint produced by the present invention and comparative example is detected, testing result It is as shown in table 1:
Adhesive force test
Reference standard JB/T9286 is tested, and 0 grade preferably, and 1 grade is taken second place.
Impact strength test
Reference standard GB/T1732 is measured.
By the car paint even application in anti-oxidant aqueous automobile paint produced by the present invention and comparative example in tinplate On, coating thickness 2.5mm toasts 30min at 60 DEG C, the precoating plate Sample A that is prepared, B, C, D, E, F.
Dry scratch resistance test
It is coated with abrasive material thin layer on the clear coat of sample board, then puts on exceedingly beautiful felt fingerstall, resists contact sample board, carries out Round-trip 10 times wipe, scratches situation to test it.Scratch resistance is not scratched relatively by measuring the scratch region of clad plate The relative ratios of the glossiness at 20 ° of visual angles in region, i.e. gloss protect percentage to indicate.
Resistance to ag(e)ing test
It is measured according to standard GB/T1865-2009.
1 performance measurement result of table
Test item Example 1(A) Example 2(B) Example 3(C) Comparative example 1(D) Comparative example (E) Comparative example (F)
Adhesive force 0 grade 0 grade 0 grade 2 grades 1 grade 1 grade
Levelability (mm) 97 97 98 74 83 85
Curing time (min) 50 47 43 74 66 68
Dry scratch resistance (gloss retention) 97.5 97.8 98.2 84.5 90.2 93.4
20 ° of gloss 98 99 99 87 85 91
Impact strength (kgcm) 58.4 58.8 58.9 35.0 39.2 43.8
Resistance to ag(e)ing (480h) It does not corrode, is not blistering, no It peels off It does not corrode, is not blistering, no It peels off Do not corrode, is not blistering, It does not peel off It is existing to generate slight removing As It is existing to generate slight removing As It is existing to generate slight removing As
From the data in table 1, it can be seen that anti-oxidant aqueous automobile paint produced by the present invention, with fabulous mechanical performance, excellent resistance to High-temperature behavior and antioxidant effect, keep in a variety of weather conditions not loss of gloss, it is non-discolouring, do not crack, do not fall off, have wide Wealthy prospect of the application.

Claims (8)

1. a kind of preparation method of anti-oxidant aqueous automobile paint, it is characterised in that specific preparation step are as follows:
It weighs grinding product, aqueous methacrylic acid ethyl ester resin, deionized water, isocyanates, zinc chromate, triethanolamine and gathers Amide is put into reaction kettle, is increased temperature in the kettle to 65~75 DEG C, is mixed under conditions of revolving speed is 200~240r/min 80~100min discharges up to anti-oxidant aqueous automobile paint；
The specific preparation step of the grinding product are as follows:
(1) desciccate, aluminium chloride, magnesium chloride, citric acid, propanedione and dehydrated alcohol are put into three-necked flask, with stirring 3~4h is mixed with the revolving speed of 500~600r/min in device, and it is 12~16% that mass fraction is added dropwise after stirring into three-necked flask Sodium hydroxide solution adjust pH value to 11~12 obtained reaction mixtures；
(2) oxidizing gas is passed through with the rate of 120~140mL/min into reaction mixture, is continually fed into 65~75min, Three-necked flask is placed in sonic oscillation instrument after being passed through, 3~4h is vibrated under conditions of frequency is 32~36kHz, it will after oscillation Three-necked flask is placed in resistance heating set, increases jacket temperature to 110~120 DEG C, 55~65min of heated at constant temperature, is made anti- Answer slurries；
The specific preparation step of the desciccate is
(1) by bagasse and taro skin investment baking oven, dry 3~4h, throws after dry under conditions of temperature is 65~75 DEG C Entering in planetary ball mill, 60~80min of mixed grinding is made grounds travel and minces under conditions of revolving speed is 200~260r/min, Grounds travel is minced and is put into beaker with mass fraction for 8~12% hydrochloric acid, with blender with the revolving speed of 400~500r/min 2~3h is mixed, mixed solution is made；
(2) mixed solution is put into reaction kettle, nitrogen is filled with into reaction kettle, until in kettle air pressure be increased to 1.3~ 1.5MPa sealing reaction kettle, temperature in the kettle is increased to 160~180 DEG C, constant temperature and pressure reacts 2~3h and reaction solution is made, and will react Liquid investment is concentrated and dried in device, and 2~3h is concentrated and dried under conditions of vacuum degree is 100~120Pa, temperature is 55~65 DEG C Desciccate is made.
2. a kind of preparation method of anti-oxidant aqueous automobile paint according to claim 1, it is characterised in that: preferably press Parts by weight meter, the grinding product is 16~18 parts, aqueous methacrylic acid ethyl ester resin is 20~22 parts, deionized water For 26~30 parts, isocyanates be 2~3 parts, zinc chromate is 0.6~0.8 part, triethanolamine is 1~2 part, polyamide is 3~5 Part.
3. a kind of preparation method of anti-oxidant aqueous automobile paint according to claim 1, it is characterised in that: grinding product Specific preparation step (1) in it is preferred according to parts by weight, desciccate is 6~8 parts, aluminium chloride is 0.4~0.8 part, chlorine Change magnesium is 0.2~0.4 part, citric acid is 2~4 parts, propanedione is 5~7 parts, dehydrated alcohol is 13~15 parts.
4. a kind of preparation method of anti-oxidant aqueous automobile paint according to claim 1, it is characterised in that: grinding product Specific preparation step (1) described in a small amount of hydrochloric acid can further be added dropwise in three-necked flask be mixed into stirring.
5. a kind of preparation method of anti-oxidant aqueous automobile paint according to claim 1, it is characterised in that: grinding product Specific preparation step (2) described in oxidizing gas be more preferably ozone, chlorine, nitric oxide it is one such or It is a variety of to mix in any proportion.
6. a kind of preparation method of anti-oxidant aqueous automobile paint according to claim 1, it is characterised in that: desciccate Specific preparation step (1) described in the mass ratio of bagasse and taro skin be 3:1.
7. a kind of preparation method of anti-oxidant aqueous automobile paint according to claim 1, it is characterised in that: desciccate Specific preparation step (1) described in the mince mass ratio of the hydrochloric acid for being 8~12% with mass fraction of grounds travel be 1:10.
8. a kind of preparation method of anti-oxidant aqueous automobile paint according to claim 1, it is characterised in that: desciccate Specific preparation step (2) described in reaction kettle warming temperature further be preferably 172~176 DEG C.
CN201910206066.9A 2019-03-19 2019-03-19 A kind of preparation method of anti-oxidant aqueous automobile paint Withdrawn CN110093080A (en)

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CN201910206066.9A CN110093080A (en) 2019-03-19 2019-03-19 A kind of preparation method of anti-oxidant aqueous automobile paint

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