CN110527409A - A kind of preparation method of high viscosity high temperature resistant coatings for tin plate printing - Google Patents
A kind of preparation method of high viscosity high temperature resistant coatings for tin plate printing Download PDFInfo
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- CN110527409A CN110527409A CN201910679222.3A CN201910679222A CN110527409A CN 110527409 A CN110527409 A CN 110527409A CN 201910679222 A CN201910679222 A CN 201910679222A CN 110527409 A CN110527409 A CN 110527409A
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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
- C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
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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
- 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
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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
- 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
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- 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
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- 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
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- C08K2201/011—Nanostructured additives
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
The present invention relates to a kind of preparation methods of high viscosity high temperature resistant coatings for tin plate printing, belong to technical field of paint preparation.Grinding product is made using cotton and taro skin as raw material in the present invention, again with methane liquid, filtrate is obtained by filtration in soy meal mixed fermentation, SiO 2 powder is then added, reaction lotion is made, finally by enriched product and cyclohexanone, propylene glycol monomethyl ether etc. mixes up to high viscosity high temperature resistant coatings for tin plate printing, elder generation's hydrocellulose of the present invention, sugared part, generate carboxyl, hydroxyl radical free radical, enhance the bonding degree between each ingredient, oxidation processes are carried out to organic fiber again, nano-scale aluminum oxide particle is filled in cellulose, be conducive to enhance the mechanical strength and heat resistance of coatings for tin plate printing, nano grade silica particles are mixed with organic fiber, silicate component is generated to be dispersed in organic fiber, reinforce the intensity of organic fiber structure, and improve its heat resistance, keep coatings for tin plate printing chemical property more stable, it has broad application prospects.
Description
Technical field
The present invention relates to a kind of preparation methods of high viscosity high temperature resistant coatings for tin plate printing, belong to technical field of paint preparation.
Background technique
As the high speed development of China's packaging industry makes tank industry processed, there has also been huge development.Malleable iron mouth is also known as tin plating
Iron is that being commonly called as tinfoil paper steel plate is electroplated, because tinplate itself has good leakproofness, keeping quality, photophobism and robustness etc.,
It is the metal material and the common raw material of can that people are commonly used.It is widely used in packing container (tank processed, tubbing
And food and drink packaging) field.Upgrading is constantly updated in the development of iron can printing industry therewith with the needs of people, and people are to production
The requirement of product packaging also correspondinglys increase, and exquisite durable and convenient for recycling iron flask, which is packed, to be constantly used in such as cookies jar, moon cake
On the products such as box, tea can, milk pot, beverage can, inhalator jar, this development has also driven the development of coatings for tin plate printing.
Coatings for tin plate printing belongs to thermohardening lacquer, is attached to metal surface (tinplate, aluminium sheet, steel by printing or roller coating painting
Plate), then baking-curing, forms tough and tensile film.Coatings for tin plate printing also needs other than should have a degree of water repelling property
There is its special requirement, such as higher to pigmenting power and life requirement, it is relatively strong according to should also have the characteristics of tin graphed sheet
Adhesive force, good heat resistance, impact resistance, boiling resistance, light resistance and processability good (molding, punching, seam etc.) etc..
Tin graphed sheet primer base is one layer of bridging agent of tinplate Yu coating quality inspection, and effect is to keep coating or whiting firm attached
With on tinplate.
Coatings for tin plate printing is divided into interlayer coatings, outer layer coating.Outer layer coating can be divided into again outer layer base oil, printed form chalk and
Roller coating type chalk, colored ink, finishing oil etc..Dried forms have baking-type and ultraviolet curing type (UV).Baking-type, that is, thermosetting
Change type, feature are that adhesive force is good, alkali resistance is excellent, but its greatest problem is that curing rate is slow, and working time and period are long, energy
Source consumption is big, individual tin graphed sheet lacks flexibility and originality.UV coatings for tin plate printing is to make light-sensitive material molecule using ultraviolet light
It is decomposed to form overactivity atom or overactivity atomic group, these overactivity atoms and atomic group make organising containing unsaturated bond
It closes object and induces a series of light-initiated chain reaction, finally reach molecule cross-link polymerizing curable drying purpose, be the one of coatings for tin plate printing
A developing direction.Using ultraviolet light curing mode, traditional tin graphed sheet mode has been overturned completely, can be greatly reduced and is produced into for enterprise
This, improves production efficiency, reduces production cost.But the adhesive force of UV coatings for tin plate printing is poor, is not easy to carry out coloured silk on it
Draw, and alkali resistance, flexibility, in terms of performance also not as good as heat cure coatings for tin plate printing effect it is good, be easy to appear xanthochromia
Problem.
It shows as that viscosity is higher, mobility is smaller to coatings for tin plate printing in the prior art in nature, however, this is to print
The transfer of coating is very unfavorable when brush, therefore also needs to improve the printing adaptability of metal coatings for tin plate printing.In addition, on packaging material
Chemical substance not exclusively has inertia, it has the possibility migrated in food into packaging, then finally flows into human body by food,
It causes harm to the human body, improves coating composition molecular weight to prevent coatings for tin plate printing generation material transport and be necessary.
Therefore it provides a kind of coatings for tin plate printing, has faster curing and drying speed, comparing with traditional coatings for tin plate printing has
More excellent adhesive force, alkali resistance, flexibility and wearability are this field urgent problems to be solved.
Summary of the invention
The technical problems to be solved by the invention:, easy to fall off, heat-resisting quantity bad for current coatings for tin plate printing adhesive property
The insufficient defect of energy, provides a kind of preparation method of high viscosity high temperature resistant coatings for tin plate printing.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
The specific preparation step of high viscosity high temperature resistant coatings for tin plate printing are as follows:
Reaction lotion is put into Rotary Evaporators, under conditions of temperature is 60~70 DEG C and revolving speed is 500~550r/min
It is concentrated and dried 2~3h and enriched product is made, enriched product, cyclohexanone, propylene glycol monomethyl ether, ethylene glycol monobutyl ether are put into blender
In be uniformly mixed obtained modification liquid, by modification liquid and polyester resin, stirring is mixed under conditions of revolving speed is 1200~1400r/min
40~50min is closed up to high viscosity high temperature resistant coatings for tin plate printing；
React the specific preparation step of lotion are as follows:
(1) tunning is put into reaction kettle, reaction kettle is closed, nitrogen is filled with into reaction kettle until air pressure in reaction kettle
It is increased to 1.2~1.6MPa, reactor temperature is increased to 150~180 DEG C, 80~100min is reacted under the conditions of constant temperature and pressure,
Filtrate is obtained by filtration after reaction, the hydrochloric acid that filtrate and mass fraction are 5~8% is put into beaker, with blender with 400~
The revolving speed of 500r/min is mixed 30~40min and is made to reaction solution；
(2) potassium permanganate powder is added into beaker, places the beaker in the water-bath that bath temperature is 30~35 DEG C, with stirring
Device is mixed 50~60min with the revolving speed of 400~500r/min and oxidation liquid is made, by oxidation liquid and aluminium chloride
Powder is put into single-necked flask, and single-necked flask is placed in sonic oscillation instrument, and oscillation is mixed under conditions of frequency is 32~36kHz
It closes 3~4h and mixed serum is made；
(3) it will be uniformly mixed in mixed serum and nano grade silica particles investment reaction kettle, quality point be added dropwise into reaction kettle
Number adjusts pH value to 11~12 for 10~15% sodium hydroxide solution, and rear closed reactor is mixed evenly, increases reaction kettle
The hydrochloric acid tune that mass fraction is 5~8% is added dropwise to 160~180 DEG C, 1~2h of isothermal reaction in interior temperature into reaction kettle after reaction
PH value is saved to 6.0~6.5,2~3h is mixed, reaction lotion is made；
The specific preparation step of tunning are as follows:
(1) it will be pulverized and mixed to obtain mixed material in cotton and taro skin investment pulverizer, successively be washed with acetone and dehydrated alcohol
It washs mixed material 3~5 times, puts into baking oven, dry 3~4h, puts into planet after dry under conditions of temperature is 80~90 DEG C
In ball mill, 50~60min of ground and mixed is ground under conditions of ratio of grinding media to material is 10:1 and revolving speed is 300~350r/min
Product；
(2) grinding product, distilled water, methane liquid, soy meal are putted into fermenter, with blender with 500~600r/min's
20~30min is mixed in revolving speed, and fermentor opening is placed in the greenhouse that temperature is 35~38 DEG C after stirring, and constant temperature stands 4
~6 days obtained tunnings.
Preferably according to parts by weight, enriched product is 8~10 parts, cyclohexanone is 1.0~1.2 parts, propylene glycol monomethyl ether 4
~6 parts, ethylene glycol monobutyl ether be 13~15 parts.
The mass ratio of modification liquid and polyester resin is 1:4.
The mass ratio for reacting the hydrochloric acid that filtrate and mass fraction are 5~8% in the specific preparation step (1) of lotion is 1:5.
The quality for reacting the potassium permanganate powder being added in the specific preparation step (2) of lotion into beaker is to reaction solution
The mass ratio of the 8~10% of quality, oxidation liquid and aluminum chloride powder is 5:1.
Reacting the mass ratio of mixed serum and nano grade silica particles in the specific preparation step (3) of lotion is 20:1.
The mass ratio of cotton and taro skin is 5:1 in the specific preparation step (1) of tunning.
In the specific preparation step (2) of tunning preferably according to parts by weight, grinding product is 15~17 parts, distills
Water is 4~6 parts, methane liquid is 1~2 part, soy meal is 5~7 parts.
The method have the benefit that:
(1) cotton and taro skin are pulverized and mixed by the present invention first, the obtained grinding product of drying grinding, then by grinding product and natural pond
Tunning is made in gas-liquid, soy meal mixed fermentation, and tunning is then carried out high-temperature high-voltage reaction, is obtained by filtration after reaction
Filtrate and mixed in hydrochloric acid are made to reaction solution filtrate, then oxidation is made to which potassium permanganate oxidation reaction is added in reaction solution
Reaction solution, then aluminum chloride powder oscillation mixing is added into oxidation liquid, is then added SiO 2 powder, adjust pH value to
Reaction lotion is made in pyroreaction after alkalinity, enriched product then is made in reaction lotion concentration and evaporation, finally by enriched product
It is mixed with organic solvents such as cyclohexanone, propylene glycol monomethyl ethers, polyester resin is added after mixing and is mixed up to the resistance to height of high viscosity
Warm coatings for tin plate printing, cotton and taro skin are carried out microbial fermentation to the present invention and fibre therein is isolated in high temperature high pressure process extraction
Dimension element, sugar molecule, and cellulose, sugared part organic matter is made to obtain a degree of hydrolysis, carboxyl, hydroxyl radical free radical are generated, is increased
Bonding degree between strong each ingredient, cellulose form fine and close cross-linked network each other, are conducive to improve coatings for tin plate printing
Mechanical strength, sugar hydrolysis generate small molecule carbohydrate molecule, further increase coating internal bond degree and coating to extraneous base
The adhesion strength of material enhances the adhesion strength of coatings for tin plate printing, then carries out oxidation processes to organic fiber, makes hydroxyl therein certainly
It is aoxidized by base and generates carboxyl free radical, the carboxyl free radical Absorptive complex wave aluminium ion of generation, aluminium ion passes through and sodium hydroxide root
Ionic reaction generates aluminium hydroxide, generates alumina in Nano level using high temperature boiling, nano-scale aluminum oxide particle is filled in fibre
In dimension element, be conducive to the mechanical strength and heat resistance that enhance coatings for tin plate printing；
(2) present invention mixes nano grade silica particles with organic fiber, by lye pyroreaction, generates silicate component
It is dispersed in organic fiber, pH value is adjusted after silicate mixing and generates silicic acid, silicic acid, which further decomposes, generates silica
And water, nanosized silica particles are dispersed in organic principle, are filled in organic fibre pipe, and organic fiber structure is reinforced
Intensity, and improve its heat resistance, to further enhance the mechanical property and heat resistance of coatings for tin plate printing, keep coatings for tin plate printing difficult
To fall off, chemical property is more stable, has broad application prospects.
Specific embodiment
It will be pulverized and mixed to obtain mixed material in cotton and taro skin 5:1 in mass ratio investment pulverizer, successively use acetone
It washs mixed material 3~5 times, is put into baking oven with dehydrated alcohol, dry 3~4h, does under conditions of temperature is 80~90 DEG C
It is dry after investment planetary ball mill in, under conditions of ratio of grinding media to material is 10:1 and revolving speed is 300~350r/min ground and mixed 50~
60min obtains grinding product；According to parts by weight, by 15~17 parts of above-mentioned grinding products, 4~6 parts of distilled water, 1~2 part of biogas
Liquid, 5~7 parts of soy meals put into fermenter, and 20~30min is mixed with the revolving speed of 500~600r/min with blender, stirs
Fermentor opening is placed in the greenhouse that temperature is 35~38 DEG C after mixing, constant temperature stands 4~6 days obtained tunnings；It will be above-mentioned
Tunning is put into reaction kettle, and reaction kettle is closed, and nitrogen is filled with into reaction kettle until air pressure is increased to 1.2 in reaction kettle
~1.6MPa increases reactor temperature to 150~180 DEG C, 80~100min is reacted under the conditions of constant temperature and pressure, is filtered after reaction
Obtain filtrate, the hydrochloric acid 1:5 in mass ratio that filtrate and mass fraction are 5~8% put into beaker, with blender with 400~
The revolving speed of 500r/min is mixed 30~40min and is made to reaction solution；Into above-mentioned beaker be added to reaction solution quality 8~
10% potassium permanganate powder, placing the beaker bath temperature is in 30~35 DEG C of water-bath, with agitating device with 400~
The revolving speed of 500r/min is mixed 50~60min and oxidation liquid is made, and oxidation liquid and aluminum chloride powder are pressed quality
Than single-necked flask being placed in sonic oscillation instrument, is vibrated under conditions of frequency is 32~36kHz in 5:1 investment single-necked flask
It mixes 3~4h and mixed serum is made；It is in mass ratio that 20:1 investment is reacted with nano grade silica particles by above-mentioned mixed serum
It is uniformly mixed in kettle, the sodium hydroxide solution that mass fraction is 10~15% is added dropwise into reaction kettle and adjusts pH value to 11~12, mixes
Closed reactor after mixing evenly is closed, increases reactor temperature to 160~180 DEG C, 1~2h of isothermal reaction, to anti-after reaction
It answers the salt acid for adjusting pH value that dropwise addition mass fraction is 5~8% in kettle to 6.0~6.5,2~3h is mixed, reaction lotion is made；
Above-mentioned reaction lotion is put into Rotary Evaporators, under conditions of temperature is 60~70 DEG C and revolving speed is 500~550r/min
Be concentrated and dried 2~3h be made enriched product, according to parts by weight, by 8~10 parts of enriched products, 1.0~1.2 parts of cyclohexanone, 4~
Modification liquid is uniformly made in 6 parts of propylene glycol monomethyl ethers, 13~15 parts of ethylene glycol monobutyl ether investment blender and mixings, by modification liquid and gathers
It is resistance to up to high viscosity that ester resin 1:4 in mass ratio is stirred 40~50min under conditions of revolving speed is 1200~1400r/min
High temperature coatings for tin plate printing.
Embodiment 1
The preparation of grinding product:
It will be pulverized and mixed to obtain mixed material in cotton and taro skin 5:1 in mass ratio investment pulverizer, successively use acetone and nothing
Water-ethanol washs mixed material 3 times, puts into baking oven, and dry 3h under conditions of temperature is 80 DEG C puts into planet ball after dry
In grinding machine, ground and mixed 50min obtains grinding product under conditions of ratio of grinding media to material is 10:1 and revolving speed is 300r/min.
The preparation of tunning:
According to parts by weight, 15 parts of above-mentioned grinding products, 4 parts of distilled water, 1 part of methane liquid, 5 parts of soy meals are put into fermentor
In, 20min is mixed with the revolving speed of 500r/min with blender, fermentor opening is placed in the temperature that temperature is 35 DEG C after stirring
In room, constant temperature stands 4 days obtained tunnings.
Preparation to reaction solution:
Above-mentioned tunning is put into reaction kettle, reaction kettle is closed, nitrogen is filled with into reaction kettle up to gas in reaction kettle
Pressure is increased to 1.2MPa, increases reactor temperature to 150 DEG C, 80min is reacted under the conditions of constant temperature and pressure, is obtained by filtration after reaction
Filtrate puts into the hydrochloric acid 1:5 in mass ratio that filtrate and mass fraction are 5% in beaker, with blender with the revolving speed of 400r/min
30min is mixed to be made to reaction solution.
The preparation of mixed serum:
The potassium permanganate powder to reaction solution quality 8% is added into above-mentioned beaker, places the beaker the water that bath temperature is 30 DEG C
In bath, 50min is mixed with the revolving speed of 400r/min with agitating device, oxidation liquid is made, by oxidation liquid and chlorine
Change in aluminium powder 5:1 in mass ratio investment single-necked flask, single-necked flask is placed in sonic oscillation instrument, is 32kHz's in frequency
Under the conditions of oscillation mixing 3h be made mixed serum.
React the preparation of lotion:
It is in mass ratio to be uniformly mixed in 20:1 investment reaction kettle with nano grade silica particles by above-mentioned mixed serum, Xiang Fanying
The sodium hydroxide solution that mass fraction is 10% is added dropwise in kettle and adjusts pH value to 11, rear closed reactor is mixed evenly, increases
The salt acid for adjusting pH value that mass fraction is 5% is added dropwise to 160 DEG C, isothermal reaction 1h in reactor temperature into reaction kettle after reaction
To 6.0,2h is mixed, reaction lotion is made.
The preparation of high viscosity high temperature resistant coatings for tin plate printing:
Above-mentioned reaction lotion is put into Rotary Evaporators, concentration is dry under conditions of temperature is 60 DEG C and revolving speed is 500r/min
Enriched product is made in dry 2h, according to parts by weight, by 8 parts of enriched products, 1.0 parts of cyclohexanone, 4 parts of propylene glycol monomethyl ethers, 13 parts of second
Glycol monobutyl ether puts into blender and mixing and modification liquid is uniformly made, by modification liquid and polyester resin 1:4 in mass ratio in revolving speed
To be stirred 40min under conditions of 1200r/min up to high viscosity high temperature resistant coatings for tin plate printing.
Embodiment 2
The preparation of grinding product:
It will be pulverized and mixed to obtain mixed material in cotton and taro skin 5:1 in mass ratio investment pulverizer, successively use acetone and nothing
Water-ethanol washs mixed material 4 times, puts into baking oven, and dry 3h under conditions of temperature is 85 DEG C puts into planet ball after dry
In grinding machine, ground and mixed 55min obtains grinding product under conditions of ratio of grinding media to material is 10:1 and revolving speed is 325r/min.
The preparation of tunning:
According to parts by weight, 16 parts of above-mentioned grinding products, 5 parts of distilled water, 1 part of methane liquid, 6 parts of soy meals are put into fermentor
In, 25min is mixed with the revolving speed of 550r/min with blender, fermentor opening is placed in the temperature that temperature is 37 DEG C after stirring
In room, constant temperature stands 5 days obtained tunnings.
Preparation to reaction solution:
Above-mentioned tunning is put into reaction kettle, reaction kettle is closed, nitrogen is filled with into reaction kettle up to gas in reaction kettle
Pressure is increased to 1.4MPa, increases reactor temperature to 170 DEG C, 90min is reacted under the conditions of constant temperature and pressure, is obtained by filtration after reaction
Filtrate puts into the hydrochloric acid 1:5 in mass ratio that filtrate and mass fraction are 6% in beaker, with blender with the revolving speed of 450r/min
35min is mixed to be made to reaction solution.
The preparation of mixed serum:
The potassium permanganate powder to reaction solution quality 9% is added into above-mentioned beaker, places the beaker the water that bath temperature is 33 DEG C
In bath, 55min is mixed with the revolving speed of 450r/min with agitating device, oxidation liquid is made, by oxidation liquid and chlorine
Change in aluminium powder 5:1 in mass ratio investment single-necked flask, single-necked flask is placed in sonic oscillation instrument, is 34kHz's in frequency
Under the conditions of oscillation mixing 3h be made mixed serum.
React the preparation of lotion:
It is in mass ratio to be uniformly mixed in 20:1 investment reaction kettle with nano grade silica particles by above-mentioned mixed serum, Xiang Fanying
The sodium hydroxide solution that mass fraction is 13% is added dropwise in kettle and adjusts pH value to 11, rear closed reactor is mixed evenly, increases
The salt acid for adjusting pH value that mass fraction is 7% is added dropwise to 170 DEG C, isothermal reaction 1h in reactor temperature into reaction kettle after reaction
To 6.3,2h is mixed, reaction lotion is made.
The preparation of high viscosity high temperature resistant coatings for tin plate printing:
Above-mentioned reaction lotion is put into Rotary Evaporators, concentration is dry under conditions of temperature is 65 DEG C and revolving speed is 525r/min
Enriched product is made in dry 2h, according to parts by weight, by 9 parts of enriched products, 1.1 parts of cyclohexanone, 5 parts of propylene glycol monomethyl ethers, 14 parts of second
Glycol monobutyl ether puts into blender and mixing and modification liquid is uniformly made, by modification liquid and polyester resin 1:4 in mass ratio in revolving speed
To be stirred 45min under conditions of 1300r/min up to high viscosity high temperature resistant coatings for tin plate printing.
Embodiment 3
The preparation of grinding product:
It will be pulverized and mixed to obtain mixed material in cotton and taro skin 5:1 in mass ratio investment pulverizer, successively use acetone and nothing
Water-ethanol washs mixed material 5 times, puts into baking oven, and dry 4h under the conditions of at a temperature of 90 °C puts into planet ball after dry
In grinding machine, ground and mixed 60min obtains grinding product under conditions of ratio of grinding media to material is 10:1 and revolving speed is 350r/min.
The preparation of tunning:
According to parts by weight, 17 parts of above-mentioned grinding products, 6 parts of distilled water, 2 parts of methane liquids, 7 parts of soy meals are put into fermentor
In, 30min is mixed with the revolving speed of 600r/min with blender, fermentor opening is placed in the temperature that temperature is 38 DEG C after stirring
In room, constant temperature stands 6 days obtained tunnings.
Preparation to reaction solution:
Above-mentioned tunning is put into reaction kettle, reaction kettle is closed, nitrogen is filled with into reaction kettle up to gas in reaction kettle
Pressure is increased to 1.6MPa, increases reactor temperature to 180 DEG C, 100min is reacted under the conditions of constant temperature and pressure, is filtered after reaction
To filtrate, the hydrochloric acid 1:5 in mass ratio that filtrate and mass fraction are 8% is put into beaker, with blender turning with 500r/min
Speed is mixed 40min and is made to reaction solution.
The preparation of mixed serum:
The potassium permanganate powder to reaction solution quality 10% is added into above-mentioned beaker, placing the beaker bath temperature is 35 DEG C
In water-bath, 60min is mixed with the revolving speed of 500r/min with agitating device, oxidation liquid is made, by oxidation liquid with
Aluminum chloride powder 5:1 in mass ratio is put into single-necked flask, and single-necked flask is placed in sonic oscillation instrument, is 36kHz in frequency
Under conditions of oscillation mixing 4h be made mixed serum.
React the preparation of lotion:
It is in mass ratio to be uniformly mixed in 20:1 investment reaction kettle with nano grade silica particles by above-mentioned mixed serum, Xiang Fanying
The sodium hydroxide solution that mass fraction is 15% is added dropwise in kettle and adjusts pH value to 12, rear closed reactor is mixed evenly, increases
The salt acid for adjusting pH value that mass fraction is 8% is added dropwise to 180 DEG C, isothermal reaction 2h in reactor temperature into reaction kettle after reaction
To 6.5,3h is mixed, reaction lotion is made.
The preparation of high viscosity high temperature resistant coatings for tin plate printing:
Above-mentioned reaction lotion is put into Rotary Evaporators, concentration is dry under conditions of temperature is 70 DEG C and revolving speed is 550r/min
Enriched product is made in dry 3h, according to parts by weight, by 10 parts of enriched products, 1.2 parts of cyclohexanone, 6 parts of propylene glycol monomethyl ethers, 15 parts of second
Glycol monobutyl ether puts into blender and mixing and modification liquid is uniformly made, by modification liquid and polyester resin 1:4 in mass ratio in revolving speed
To be stirred 50min under conditions of 1400r/min up to high viscosity high temperature resistant coatings for tin plate printing.
Comparative example 1: it is essentially identical with the preparation method of example 1, it has only the difference is that not being added to reaction solution.
Comparative example 2: it is essentially identical with the preparation method of example 2, it has only the difference is that reaction lotion is not added.
Comparative example 3: the coatings for tin plate printing of company, Shenzhen production.
Coatings for tin plate printing in high viscosity high temperature resistant coatings for tin plate printing produced by the present invention and comparative example is detected, detection knot
Fruit is as shown in table 1:
Adhesive force test
It is measured according to JG/T24-2000 method, 0 grade preferably, and 1 grade is taken second place.
Hardness test
The hardness of coating sample is tested by pencil hardness test, the top of pencil-lead is contacted with sample surfaces, with constant speed
(0.5mm/sec) swing handle is spent, moves horizontally sample at pencil-lead opposite direction about 3mm, draws sample with pencil-lead
Surface rotates 90 ° of change directions of sample, draws in total 5 times, the pencil need to meet the requirement of JISS6006.
1 performance measurement result of table
| Test item | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Appearance of film | It is flat and smooth | It is flat and smooth | It is flat and smooth | It is flat and smooth | It is smooth | It is smooth |
| Viscosity (25 DEG C, mpas) | 3600 | 3615 | 3627 | 3245 | 3364 | 3193 |
| Adhesive force | 1 grade | 1 grade | 0 grade | 2 grades | 1 grade | 2 grades |
| Glossiness (%) | 96.7 | 97.5 | 97.8 | 84.3 | 85.6 | 80.2 |
| Hardness (pencil) | 5H | 5H | 6H | 3H | 4H | 4H |
| Heat-resisting quantity (50 DEG C, for 24 hours) | Without significant change | Without significant change | Without significant change | Without significant change | Coating is cracked | Coating is cracked |
| Water resistance (for 24 hours) | Coating is without peeling, discoloration | Coating is without peeling, discoloration | Coating is without peeling, discoloration | There is small area peeling in coating | Coating is without peeling, discoloration | There is large area peeling in coating |
| Impact resistance (Nm) | 5.1 | 5.3 | 5.4 | 4.3 | 4.6 | 4.5 |
From the data in table 1, it can be seen that high viscosity high temperature resistant coatings for tin plate printing produced by the present invention, strength of coating is high, has preferable attachment
Power, water resistance, high temperature resistance and impact resistance are excellent, and environment-protecting and non-poisonous, and stability is good, before wide application
Scape.
Claims (8)
1. a kind of preparation method of high viscosity high temperature resistant coatings for tin plate printing, it is characterised in that specific preparation step are as follows:
Reaction lotion is put into Rotary Evaporators, under conditions of temperature is 60~70 DEG C and revolving speed is 500~550r/min
It is concentrated and dried 2~3h and enriched product is made, enriched product, cyclohexanone, propylene glycol monomethyl ether, ethylene glycol monobutyl ether are put into blender
In be uniformly mixed obtained modification liquid, by modification liquid and polyester resin, stirring is mixed under conditions of revolving speed is 1200~1400r/min
40~50min is closed up to high viscosity high temperature resistant coatings for tin plate printing；
The specific preparation step of the reaction lotion are as follows:
(1) tunning is put into reaction kettle, reaction kettle is closed, nitrogen is filled with into reaction kettle until air pressure in reaction kettle
It is increased to 1.2~1.6MPa, reactor temperature is increased to 150~180 DEG C, 80~100min is reacted under the conditions of constant temperature and pressure,
Filtrate is obtained by filtration after reaction, the hydrochloric acid that filtrate and mass fraction are 5~8% is put into beaker, with blender with 400~
The revolving speed of 500r/min is mixed 30~40min and is made to reaction solution；
(2) potassium permanganate powder is added into beaker, places the beaker in the water-bath that bath temperature is 30~35 DEG C, with stirring
Device is mixed 50~60min with the revolving speed of 400~500r/min and oxidation liquid is made, by oxidation liquid and aluminium chloride
Powder is put into single-necked flask, and single-necked flask is placed in sonic oscillation instrument, and oscillation is mixed under conditions of frequency is 32~36kHz
It closes 3~4h and mixed serum is made；
(3) it will be uniformly mixed in mixed serum and nano grade silica particles investment reaction kettle, quality point be added dropwise into reaction kettle
Number adjusts pH value to 11~12 for 10~15% sodium hydroxide solution, and rear closed reactor is mixed evenly, increases reaction kettle
The hydrochloric acid tune that mass fraction is 5~8% is added dropwise to 160~180 DEG C, 1~2h of isothermal reaction in interior temperature into reaction kettle after reaction
PH value is saved to 6.0~6.5,2~3h is mixed, reaction lotion is made；
The specific preparation step of the tunning are as follows:
(1) it will be pulverized and mixed to obtain mixed material in cotton and taro skin investment pulverizer, successively be washed with acetone and dehydrated alcohol
It washs mixed material 3~5 times, puts into baking oven, dry 3~4h, puts into planet after dry under conditions of temperature is 80~90 DEG C
In ball mill, 50~60min of ground and mixed is ground under conditions of ratio of grinding media to material is 10:1 and revolving speed is 300~350r/min
Product；
(2) grinding product, distilled water, methane liquid, soy meal are putted into fermenter, with blender with 500~600r/min's
20~30min is mixed in revolving speed, and fermentor opening is placed in the greenhouse that temperature is 35~38 DEG C after stirring, and constant temperature stands 4
~6 days obtained tunnings.
2. a kind of preparation method of high viscosity high temperature resistant coatings for tin plate printing according to claim 1, it is characterised in that: preferred
According to parts by weight, the enriched product is 8~10 parts, cyclohexanone is 1.0~1.2 parts, propylene glycol monomethyl ether is 4~6 parts, second
Glycol monobutyl ether is 13~15 parts.
3. a kind of preparation method of high viscosity high temperature resistant coatings for tin plate printing according to claim 1, it is characterised in that: described
The mass ratio of modification liquid and polyester resin is 1:4.
4. a kind of preparation method of high viscosity high temperature resistant coatings for tin plate printing according to claim 1, it is characterised in that: reaction cream
The mass ratio for the hydrochloric acid that filtrate described in the specific preparation step (1) of liquid and mass fraction are 5~8% is 1:5.
5. a kind of preparation method of high viscosity high temperature resistant coatings for tin plate printing according to claim 1, it is characterised in that: reaction cream
The quality for the potassium permanganate powder being added described in the specific preparation step (2) of liquid into beaker is 8 to reaction solution quality
~10%, the mass ratio of oxidation liquid and aluminum chloride powder is 5:1.
6. a kind of preparation method of high viscosity high temperature resistant coatings for tin plate printing according to claim 1, it is characterised in that: reaction cream
The mass ratio of mixed serum described in the specific preparation step (3) of liquid and nano grade silica particles is 20:1.
7. a kind of preparation method of high viscosity high temperature resistant coatings for tin plate printing according to claim 1, it is characterised in that: fermentation produces
The mass ratio of cotton described in the specific preparation step (1) of object and taro skin is 5:1.
8. a kind of preparation method of high viscosity high temperature resistant coatings for tin plate printing according to claim 1, it is characterised in that: fermentation produces
In the specific preparation step (2) of object preferably according to parts by weight, the grinding product is 15~17 parts, distilled water is 4~6
Part, methane liquid are 1~2 part, soy meal is 5~7 parts.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111171271A (en) * | 2020-02-25 | 2020-05-19 | 吴超群 | Preparation method of heat-resistant polyurethane elastomer |
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| CN106151467A (en) * | 2015-04-30 | 2016-11-23 | 高旋 | A kind of aluminium alloy gear box |
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Cited By (2)
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| CN111171271A (en) * | 2020-02-25 | 2020-05-19 | 吴超群 | Preparation method of heat-resistant polyurethane elastomer |
| CN111171271B (en) * | 2020-02-25 | 2022-08-19 | 广州市环友高分子新材料有限公司 | Preparation method of heat-resistant polyurethane elastomer |
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