CN109971347A - A kind of preparation method of high viscosity high intensity raw lacquer - Google Patents
A kind of preparation method of high viscosity high intensity raw lacquer Download PDFInfo
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- CN109971347A CN109971347A CN201910165895.7A CN201910165895A CN109971347A CN 109971347 A CN109971347 A CN 109971347A CN 201910165895 A CN201910165895 A CN 201910165895A CN 109971347 A CN109971347 A CN 109971347A
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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
- C09D193/00—Coating compositions based on natural resins; Coating compositions based on derivatives thereof
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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
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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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
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Abstract
The invention discloses a kind of preparation methods of high viscosity high intensity raw lacquer, belong to technical field of paint preparation.The present invention is dry by sawdust and stalk first, ground and mixed, mixed serum is made with hydrochloric acid impregnation after grinding, then mixed serum is subjected to high temperature high pressure process and reaction hydrolyzate is made, then reaction hydrolyzate and methane liquid are putted into fermenter and carry out the obtained tunning that ferments, tunning is subjected to microwave treatment again, aluminum sulfate is added after microwave treatment to be mixed, it is concentrated and dried after stirring and desciccate is made, by desciccate, it is stirred evenly in graphite flake investment sulfuric acid solution, add potassium permanganate reaction, filter cake is obtained by filtration after reaction, finally by filter cake, raw lacquer liquid and other auxiliary agents are stirred up to high viscosity high intensity raw lacquer.
Description
Technical field
The invention discloses a kind of preparation methods of high viscosity high intensity raw lacquer, belong to technical field of paint preparation.
Background technique
Raw lacquer using with a history of thousands of years, is known as the good reputation of " king of coating " in China.Raw lacquer is uniquely in biology
Under enzyme catalysis, completes biotransformation, spontaneously dries the natural resin coating to form a film.Raw lacquer paint film bright in color is gorgeous
Beautiful, durability, anticorrosive, solvent resistant and insulation performance are splendid.Raw lacquer has been used as excellent decoration and protection materials, is widely applied
In industries such as petroleum, chemical industry, weaving, printing and dyeing, craftwork and top-grade furnitures.But raw lacquer membrance casting condition is more harsh, it is necessary to one
Determine ability drying and forming-film under temperature and humidity, paint film uvioresistant absorbent properties are not good enough, are easy aging cracking outdoors;Meanwhile
That there is also paint film alkali resistances is poor, is not easy to spray, has the drawbacks such as sensitization, to affect the development of raw lacquer industrially.Laccol
It is the main film forming substance of raw lacquer, the catechol group containing unsaturated terminal chain in molecular structure has multiple reactivities
The series reactions such as esterification, etherificate, alkylation, complexing, polycondensation, copolymerization can occur for center.Recent domestic is to raw lacquer
Membrane formation mechanism and modification have made intensive studies.Raw lacquer passes through the modified coating that a variety of suitable different demands can not only be made
Product reduces the usage amount of raw lacquer, realizes higher economic benefit, moreover it is possible to the functional material for obtaining some superior performances, from
And the application field of raw lacquer is expanded.
Raw lacquer is white thick liquid, is a kind of water-in-oil emulsion, and main component is laccol, laccase, gumminess and water
Point etc..Raw lacquer is not widely applied but as coating so far, this is primarily due to raw lacquer, and there is some shortcomings, such as
Raw lacquer must (relative humidity is not less than 80%, and temperature is 20~30 DEG C) ability film-forming, and raw lacquer under given conditions
There is sensitization and slow drying speed to part population, these deficiencies limit the popularization and application of raw lacquer.
Raw lacquer drying and forming-film mainly relies on Laccase Catalyzed oxidation laccol polymerization, and process is also along with unsaturated long side chain
Autoxidation polymerization, but its reaction be very slowly.However, the catalytic activity of laccase is influenced by many environmental factors, such as
Laccase will inactivate when temperature is more than 60 DEG C, and laccase activity also can gradually weaken as the resting period increases, so as to cause life
Qi Buneng is certainly dry.Currently, being applied for preparation synthesis after cannot mainly extracting laccol using organic solvent from dry raw lacquer application
Material, this has abandoned the natural characteristic of raw lacquer and will cause environmental pollution.Also research urges to laccase cannot being added from dry raw lacquer
Agent restores its film performance, but laccase extraction cost is very expensive, and is unfavorable for its extensive use.In addition, there are also study
It is added in not dry raw lacquer using some monokaryon bivalent cupric ions substitution laccase and promotes its film-forming, although some synthesis compounds
Show the catalytic activity of similar laccase, but they remain problem in terms of some environment.
The modification of raw lacquer is mainly to utilize the reactivity of laccol, prepares the modified raw lacquer with different function characteristic.Most
Early raw lacquer method of modifying exactly mixes tung oil, such as famous " wide paint ", " gold lacquer " in raw lacquer.Manufactured product compensates for
The deficiencies of raw lacquer paint film is thin and brittle, brightness is weak, pigment weight.In addition to tung oil, other drying oil such as linseed oil, Chinese tallow tree benevolence oil and purple perilla
Seed oil etc. can also be used for the modification of raw lacquer.But existing raw lacquer still has some problems, if wearability is bad, slow drying speed
The problems such as.
Therefore, inventing the raw lacquer that a kind of wearability is good and rate of drying is fast is necessary to technical field of paint preparation
's.
Summary of the invention
The technical problems to be solved by the invention:, differences in viscosity slow for current raw lacquer solidification rate, wear-resisting property after solidification
Bad defect provides a kind of preparation method of high viscosity high intensity raw lacquer.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
2. a kind of high viscosity high intensity raw lacquer the preparation method comprises the following steps:
3. filter cake is obtained by filtration in oxidation liquid, successively cleaned filter cake 3~5 times with dehydrated alcohol and distilled water, by filter cake, life
Paint solution, manganese naphthenate, ethylene glycol are put into high speed disperser, are mixed under conditions of revolving speed is 1200~1300r/min
Prefabricated mixed liquor is made in 15~20min, according to parts by weight, by prefabricated mixed liquor, SiO 2 powder, silane coupling agent and matter
It measures the acetum that score is 4~8% and puts into blender and mixing uniformly up to high viscosity high intensity raw lacquer；
4. the preparation of oxidation liquid:
(1) pH value is adjusted to 10~11, with stirring to the sodium hydroxide solution that mixed solution and dripping mass fraction is 3~5%
30~40min is mixed with the revolving speed of 300~400r/min in device, pours into beaker after stirring, places the beaker bath temperature
For in 95~100 DEG C of water-baths, the salt acid for adjusting pH value that mass fraction is 5~8% is added dropwise into beaker by constant temperature 2~3h of boiling
To neutrality；
(2) it places the beaker in vacuum oven, it is dry under conditions of temperature is 50~60 DEG C and vacuum degree is 80~100Pa
10~12h obtains drying composite, and the sulfuric acid solution investment that desciccate, graphite flake and mass fraction are 30~40% is placed in
It is uniformly mixed and is made to reaction solution in the beaker of ice-water bath, potassium permanganate powder is added into three-necked flask, with blender with 200
The revolving speed of~240r/min is mixed 50~60min and oxidation liquid is made；
5. the preparation of mixed solution:
(1) sawdust and agricultural crop straw are put into baking oven, dry 5~6h under conditions of temperature is 70~80 DEG C, after dry
It puts into planetary ball mill, 2~3h is ground under conditions of ratio of grinding media to material is 10:1 and revolving speed is 150~180r/min, is ground
Mixture is ground, the hydrochloric acid that milled mixtures and mass fraction are 4~8% is put into beaker, with agitating device with 300~400r/
45~60min is mixed under conditions of min, mixed serum is made；
(2) mixed serum is put into reaction kettle, nitrogen is filled with into reaction kettle until in reaction kettle air pressure be increased to 1.6~
2.0MPa increases reactor temperature to 160~180 DEG C, and mass fraction is added dropwise thereto and is by 60~80min of constant temperature and pressure reaction
3~6% sodium bicarbonate solution adjusts pH value to neutrality, reaction hydrolyzate is made, by reaction hydrolyzate and methane liquid investment fermentation
In tank；
(3) fermentor is sealed, is placed in the greenhouse that ambient temperature is 32~36 DEG C, constant temperature stands 5~7 days, obtains after standing
Tunning is placed in microwave equipment by tunning, in lift apparatus temperature to 120~140 DEG C, constant temperature stands 30~
Microwave reaction liquid is made in 40min, will be uniformly mixed to obtain mixed solution in microwave reaction liquid and Aluminium Sulphate usp (powder) investment beaker.
According to parts by weight, filter cake is 8~10 parts, raw lacquer liquid is 23~25 parts, manganese naphthenate is 1.0~1.2 parts, second two
Alcohol is 2~3 parts.
According to parts by weight, prefabricated mixed liquor is 35~37 parts, SiO 2 powder is 1~3 part, silane coupling agent 2
~4 parts, mass fraction be 4~8% acetum be 4~6 parts.
In the preparation of oxidation liquid according to parts by weight, desciccate is 6~8 parts, graphite flake is 2~3 parts, quality point
Number is 12~16 parts for 30~40% sulfuric acid solution.
The quality for the potassium permanganate powder being added in the preparation of oxidation liquid into three-necked flask is to reaction solution quality
4~6%.
The mass ratio of sawdust and agricultural crop straw is 3:1 in the preparation of mixed solution.
The mass ratio for the hydrochloric acid that milled mixtures and mass fraction are 4~8% in the preparation of mixed solution is 1:10.
The mass ratio that hydrolyzate and methane liquid are reacted in the preparation of mixed solution is 15:1.
The mass ratio of microwave reaction liquid and Aluminium Sulphate usp (powder) is 15:1 in the preparation of mixed solution.
The method have the benefit that:
15.(1) the present invention dry, ground and mixed by sawdust and stalk first, is made mixing slurry with hydrochloric acid impregnation after grinding
Then mixed serum is carried out high temperature high pressure process and reaction hydrolyzate is made by liquid, then will reaction hydrolyzate and methane liquid investment
The obtained tunning that ferments is carried out in fermentor, then tunning is subjected to microwave treatment, and it is mixed that aluminum sulfate is added after microwave treatment
Stirring is closed, is concentrated and dried after stirring and desciccate is made, will be stirred evenly in desciccate, graphite flake investment sulfuric acid solution, then
Potassium permanganate reaction is added, filter cake is obtained by filtration after reaction, is finally stirred filter cake, raw lacquer liquid and other auxiliary agents to obtain the final product
Sawdust and agricultural crop straw are passed through acid soak and high temperature high pressure process, isolate it by high viscosity high intensity raw lacquer, the present invention
In the lignin component and cellulose components that have, there is a large amount of hydroxyl radical free radical in lignin and cellulose, raw lacquer is added
In help to form Hydrogen Binding Adsorption in raw lacquer between each ingredient, improve the crosslink density of each ingredient inside raw lacquer, solidify raw lacquer
Mechanical property enhancing afterwards, while the viscosity of raw lacquer can also be improved, lignin, cellulose are also carried out microbial fermentation by the present invention
Lignin and cellulose are further decomposed in processing, reduce the carbon chain lengths of both ingredients, expand the specific surface area of organic matter,
It is exposed to more organo-functional groups outer, increases contact probability, further increase the viscosity of raw lacquer；
(2) aluminium ion is introduced into lignin and cellulose by the present invention, is attracted using aluminum ions positive and negative charge, is reinforced raw lacquer
Bond effect between Adhesion property and internal each molecule is to enhance the viscosity and mechanical property of raw lacquer, then by graphite flake and organic
Ingredient mixing, puts into and passes through potassium permanganate oxidation in sulfuric acid solution, keep lignin, cellulose and graphene oxide full cross-linked,
Graphene oxide has good thermal conduction effect, and can speed up heat transfer in solidification aggravates moisture molecular motion, promotes life
Curing rate is painted, while can also effectively enhance the wear-resisting property of raw lacquer, while the oxidation of part functional group generates carboxylic in organic principle
Base group, carboxylic group are conducive to the metal ion of complexing metal material surface, raw lacquer are made more easily to be adsorbed in metal material
On, carboxylic group is also easy to adsorbed water molecule, facilitates the conduction of hydrone and hydrone is made to come into full contact with grapheme material, make
Hydrone, which is more quickly heated, to volatilize, to improve volatilization solidification rate, has broad application prospects.
Specific embodiment
Sawdust and agricultural crop straw 3:1 in mass ratio are put into baking oven, dry 5 under conditions of temperature is 70~80 DEG C
~6h puts into planetary ball mill after dry, 2 is ground under conditions of ratio of grinding media to material is 10:1 and revolving speed is 150~180r/min
~3h, obtains milled mixtures, and the hydrochloric acid 1:10 in mass ratio that milled mixtures and mass fraction are 4~8% is put into beaker
In, mixed serum is made so that 45~60min to be mixed under the speed conditions of 300~400r/min with agitating device；It will be above-mentioned
Mixed serum put into reaction kettle in, be filled with into reaction kettle nitrogen until reaction kettle in air pressure be increased to 1.6~2.0MPa, increase
To 160~180 DEG C, constant temperature and pressure reacts 60~80min and the carbonic acid that mass fraction is 3~6% is added dropwise thereto reactor temperature
Hydrogen sodium solution adjusts pH value to neutrality, reaction hydrolyzate is made, by reaction hydrolyzate and methane liquid 15:1 in mass ratio investment hair
In fermentation tank；Above-mentioned fermentor is sealed, is placed in the greenhouse that ambient temperature is 32~36 DEG C, constant temperature stands 5~7 days, after standing
Obtain tunning, tunning be placed in microwave equipment, in lift apparatus temperature to 120~140 DEG C, constant temperature stands 30~
Microwave reaction liquid is made in 40min, will be uniformly mixed in microwave reaction liquid and Aluminium Sulphate usp (powder) 15:1 in mass ratio investment beaker
To mixed solution；To the sodium hydroxide solution that above-mentioned mixed solution and dripping mass fraction is 3~5% adjust pH value to 10~
11,30~40min is mixed with the revolving speed of 300~400r/min with blender, pours into beaker, places the beaker after stirring
In the water-bath that bath temperature is 95~100 DEG C, the hydrochloric acid that mass fraction is 5~8% is added dropwise into beaker by constant temperature 2~3h of boiling
PH value is adjusted to neutrality；Above-mentioned beaker is placed in a vacuum drying oven, in temperature be 50~60 DEG C and vacuum degree is 80~100Pa
Under conditions of dry 10~12h, drying composite is obtained, according to parts by weight, by 6~8 parts of desciccates, 2~3 parts of graphite flakes
The sulfuric acid solution for being 30~40% with 12~16 parts of mass fractions puts into the beaker of ice-water bath to be uniformly mixed and be made to reaction solution,
The potassium permanganate powder to reaction solution quality 4~6% is added into three-necked flask, with blender with the revolving speed of 200~240r/min
50~60min is mixed, oxidation liquid is made；Filter cake is obtained by filtration in above-mentioned oxidation liquid, successively with dehydrated alcohol and
Distilled water cleans filter cake 3~5 times, according to parts by weight, by 8~10 parts of filter cakes, 23~25 parts of raw lacquer liquid, 1.0~1.2 parts of cycloalkanes
In sour manganese, 2~3 parts of ethylene glycol investment high speed dispersers, it is mixed 15 under conditions of revolving speed is 1200~1300r/min~
Prefabricated mixed liquor is made in 20min, according to parts by weight, by 35~37 portions of prefabricated mixed liquors, 1~3 part of SiO 2 powder, 2~4
The acetum that part silane coupling agent and 4~6 parts of mass fractions are 4~8% puts into blender and mixing uniformly up to high viscosity height
Intensity raw lacquer.
Embodiment 1
The preparation of mixed solution:
Sawdust and agricultural crop straw 3:1 in mass ratio are put into baking oven, dry 5h under conditions of temperature is 70 DEG C, after dry
It puts into planetary ball mill, 2h is ground under conditions of ratio of grinding media to material is 10:1 and revolving speed is 150r/min, obtains milled mixtures,
The hydrochloric acid 1:10 in mass ratio that milled mixtures and mass fraction are 4% is put into beaker, with agitating device with 300r/min's
45min is mixed under speed conditions, mixed serum is made；
Above-mentioned mixed serum is put into reaction kettle, nitrogen is filled with into reaction kettle until air pressure is increased in reaction kettle
1.6MPa increases reactor temperature to 160 DEG C, and the carbon that mass fraction is 3~6% is added dropwise in constant temperature and pressure reaction 60min thereto
Sour hydrogen sodium solution adjusts pH value to neutrality, and reaction hydrolyzate is made, reaction hydrolyzate and methane liquid 15:1 in mass ratio are put into
In fermentor；
Above-mentioned fermentor is sealed, is placed in the greenhouse that ambient temperature is 32 DEG C, constant temperature stands 5 days, and fermentation is obtained after standing and is produced
Tunning is placed in microwave equipment by object, and for temperature to 120 DEG C, constant temperature stands 30min in lift apparatus, and microwave reaction is made
Liquid will be uniformly mixed to obtain mixed solution in microwave reaction liquid and Aluminium Sulphate usp (powder) 15:1 in mass ratio investment beaker；
The preparation of oxidation liquid:
Adjust pH value to 10 to the sodium hydroxide solution that above-mentioned mixed solution and dripping mass fraction is 3%, with blender with
30min is mixed in the revolving speed of 300r/min, pours into beaker after stirring, places the beaker the water-bath that bath temperature is 95 DEG C
In, constant temperature boiling 2h, the salt acid for adjusting pH value that dropwise addition mass fraction is 5% into beaker to neutrality；
Above-mentioned beaker is placed in a vacuum drying oven, dry 10h, obtains under conditions of temperature is 50 DEG C and vacuum degree is 80Pa
Drying composite, according to parts by weight, the sulfuric acid solution for being 30% by 6 parts of desciccates, 2 parts of graphite flakes and 12 parts of mass fractions
It puts into the beaker of ice-water bath to be uniformly mixed and be made to reaction solution, the permanganic acid to reaction solution quality 4% is added into three-necked flask
Potassium powder is mixed 50min with blender with the revolving speed of 200r/min and oxidation liquid is made；
The preparation of high viscosity high intensity raw lacquer:
Filter cake is obtained by filtration in above-mentioned oxidation liquid, successively cleans filter cake 3 times with dehydrated alcohol and distilled water, in parts by weight
8 parts of filter cakes, 23 parts of raw lacquer liquid, 1.0 parts of manganese naphthenates, 2 parts of ethylene glycol are put into high speed dispersers, are in revolving speed by meter
15min is mixed under conditions of 1200r/min, prefabricated mixed liquor is made, according to parts by weight, by 35 parts of prefabricated mixed liquors, 1
The acetum that part SiO 2 powder, 2 parts of silane coupling agents and 4 parts of mass fractions are 4% puts into blender and mixing and is uniformly
Obtain high viscosity high intensity raw lacquer.
Embodiment 2
The preparation of mixed solution:
By in sawdust and agricultural crop straw 3:1 in mass ratio investment baking oven, dry 5.5h, dry under conditions of temperature is 75 DEG C
It puts into planetary ball mill afterwards, 2.5h is ground under conditions of ratio of grinding media to material is 10:1 and revolving speed is 170r/min, it is mixed to obtain grinding
Object is closed, the hydrochloric acid 1:10 in mass ratio that milled mixtures and mass fraction are 6% is put into beaker, with agitating device with 350r/
55min is mixed under the speed conditions of min, mixed serum is made；
Above-mentioned mixed serum is put into reaction kettle, nitrogen is filled with into reaction kettle until air pressure is increased in reaction kettle
1.8MPa increases reactor temperature to 170 DEG C, and the carbonic acid that mass fraction is 5% is added dropwise in constant temperature and pressure reaction 70min thereto
Hydrogen sodium solution adjusts pH value to neutrality, reaction hydrolyzate is made, by reaction hydrolyzate and methane liquid 15:1 in mass ratio investment hair
In fermentation tank；
Above-mentioned fermentor is sealed, is placed in the greenhouse that ambient temperature is 34 DEG C, constant temperature stands 6 days, and fermentation is obtained after standing and is produced
Tunning is placed in microwave equipment by object, and for temperature to 130 DEG C, constant temperature stands 35min in lift apparatus, and microwave reaction is made
Liquid will be uniformly mixed to obtain mixed solution in microwave reaction liquid and Aluminium Sulphate usp (powder) 15:1 in mass ratio investment beaker；
The preparation of oxidation liquid:
Adjust pH value to 10 to the sodium hydroxide solution that above-mentioned mixed solution and dripping mass fraction is 4%, with blender with
35min is mixed in the revolving speed of 350r/min, pours into beaker after stirring, places the beaker the water-bath that bath temperature is 97 DEG C
In, constant temperature boiling 2.5h, the salt acid for adjusting pH value that dropwise addition mass fraction is 7% into beaker to neutrality；
Above-mentioned beaker is placed in a vacuum drying oven, dry 11h, obtains under conditions of temperature is 55 DEG C and vacuum degree is 90Pa
Drying composite, according to parts by weight, the sulfuric acid solution for being 35% by 7 parts of desciccates, 2 parts of graphite flakes and 14 parts of mass fractions
It puts into the beaker of ice-water bath to be uniformly mixed and be made to reaction solution, the permanganic acid to reaction solution quality 5% is added into three-necked flask
Potassium powder is mixed 55min with blender with the revolving speed of 220r/min and oxidation liquid is made；
The preparation of high viscosity high intensity raw lacquer:
Filter cake is obtained by filtration in above-mentioned oxidation liquid, successively cleans filter cake 4 times with dehydrated alcohol and distilled water, in parts by weight
9 parts of filter cakes, 24 parts of raw lacquer liquid, 1.1 parts of manganese naphthenates, 2 parts of ethylene glycol are put into high speed dispersers, are in revolving speed by meter
17min is mixed under conditions of 1250r/min, prefabricated mixed liquor is made, according to parts by weight, by 36 parts of prefabricated mixed liquors, 1
The acetum that part SiO 2 powder, 3 parts of silane coupling agents and 5 parts of mass fractions are 6% puts into blender and mixing and is uniformly
Obtain high viscosity high intensity raw lacquer.
Embodiment 3
The preparation of mixed solution:
Sawdust and agricultural crop straw 3:1 in mass ratio are put into baking oven, dry 6h under conditions of temperature is 80 DEG C, after dry
It puts into planetary ball mill, 3h is ground under conditions of ratio of grinding media to material is 10:1 and revolving speed is 180r/min, obtains milled mixtures,
The hydrochloric acid 1:10 in mass ratio that milled mixtures and mass fraction are 8% is put into beaker, with agitating device with 400r/min's
60min is mixed under speed conditions, mixed serum is made；
Above-mentioned mixed serum is put into reaction kettle, nitrogen is filled with into reaction kettle until air pressure is increased in reaction kettle
2.0MPa increases reactor temperature to 180 DEG C, and the carbonic acid that mass fraction is 6% is added dropwise in constant temperature and pressure reaction 80min thereto
Hydrogen sodium solution adjusts pH value to neutrality, reaction hydrolyzate is made, by reaction hydrolyzate and methane liquid 15:1 in mass ratio investment hair
In fermentation tank；
Above-mentioned fermentor is sealed, is placed in the greenhouse that ambient temperature is 36 DEG C, constant temperature stands 7 days, and fermentation is obtained after standing and is produced
Tunning is placed in microwave equipment by object, and for temperature to 140 DEG C, constant temperature stands 40min in lift apparatus, and microwave reaction is made
Liquid will be uniformly mixed to obtain mixed solution in microwave reaction liquid and Aluminium Sulphate usp (powder) 15:1 in mass ratio investment beaker；
The preparation of oxidation liquid:
Adjust pH value to 11 to the sodium hydroxide solution that above-mentioned mixed solution and dripping mass fraction is 5%, with blender with
40min is mixed in the revolving speed of 400r/min, pours into beaker after stirring, places the beaker the water-bath that bath temperature is 100 DEG C
In pot, constant temperature boiling 3h, the salt acid for adjusting pH value that dropwise addition mass fraction is 8% into beaker to neutrality；
Above-mentioned beaker is placed in a vacuum drying oven, dry 12h, obtains under conditions of temperature is 60 DEG C and vacuum degree is 100Pa
To drying composite, according to parts by weight, the sulfuric acid for being 40% by 8 parts of desciccates, 3 parts of graphite flakes and 16 parts of mass fractions is molten
Liquid puts into the beaker of ice-water bath to be uniformly mixed and be made to reaction solution, and the Gao Meng to reaction solution quality 6% is added into three-necked flask
Sour potassium powder is mixed 60min with blender with the revolving speed of 240r/min and oxidation liquid is made；
The preparation of high viscosity high intensity raw lacquer:
Filter cake is obtained by filtration in above-mentioned oxidation liquid, successively cleans filter cake 5 times with dehydrated alcohol and distilled water, in parts by weight
10 parts of filter cakes, 25 parts of raw lacquer liquid, 1.2 parts of manganese naphthenates, 3 parts of ethylene glycol are put into high speed dispersers, are in revolving speed by meter
20min is mixed under conditions of 1300r/min, prefabricated mixed liquor is made, according to parts by weight, by 37 parts of prefabricated mixed liquors, 3
The acetum that part SiO 2 powder, 4 parts of silane coupling agents and 6 parts of mass fractions are 8% puts into blender and mixing and is uniformly
Obtain high viscosity high intensity raw lacquer.
Comparative example 1: it is essentially identical with the preparation method of embodiment 2, it has only the difference is that lacking mixed solution.
Comparative example 2: it is essentially identical with the preparation method of embodiment 2, it has only the difference is that lacking oxidation liquid.
Comparative example 3: the high viscosity high intensity raw lacquer of Shandong company production.
Surface drying time test is detected by the standard of GB/T6753.2.
Paint film appearance test is detected by GB/T9761 standard.
Hardness of paint film test is detected by GB/1732 standard.
Example 1~3 prepared by the present invention and 1~3 sample application of comparative example are subjected to wear-resisting test on pot disk, by wearing away
Instrument tests wearability (test condition: grinding wheel CS-10, load force 500g are recycled 500 times) at room temperature, after test loop
Mass loss characterize the wearability of coating, mass loss is fewer, and the wearability of coating is better.
Adhesive force test reference standard JB/T9286 is tested, and 0 grade preferably, and 1 grade is taken second place.
Table 1: raw lacquer performance measurement result
In summary, high viscosity high intensity raw lacquer surface drying time of the invention is short as can be seen from Table 1, and dry solidification speed is fast,
Paint film appearance is flat and smooth, and hardness of paint film is high, and mass loss is low after abrasion test, and wearability is good, and adhesive force grade is high, viscosity
Height has broad prospect of application.
The foregoing is merely preferred modes of the invention, are not intended to limit the invention, all in spirit and original of the invention
Within then, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of preparation method of high viscosity high intensity raw lacquer, it is characterised in that specific preparation step are as follows:
Filter cake is obtained by filtration in oxidation liquid, is successively cleaned filter cake 3~5 times with dehydrated alcohol and distilled water, by filter cake, raw lacquer
Liquid, manganese naphthenate, ethylene glycol are put into high speed disperser, are mixed 15 under conditions of revolving speed is 1200~1300r/min
Prefabricated mixed liquor is made in~20min, according to parts by weight, by prefabricated mixed liquor, SiO 2 powder, silane coupling agent and quality
The acetum that score is 4~8% puts into blender and mixing uniformly up to high viscosity high intensity raw lacquer；
The specific preparation step of the oxidation liquid are as follows:
(1) pH value is adjusted to 10~11, with stirring to the sodium hydroxide solution that mixed solution and dripping mass fraction is 3~5%
30~40min is mixed with the revolving speed of 300~400r/min in device, pours into beaker after stirring, places the beaker bath temperature
For in 95~100 DEG C of water-baths, the salt acid for adjusting pH value that mass fraction is 5~8% is added dropwise into beaker by constant temperature 2~3h of boiling
To neutrality；
(2) it places the beaker in vacuum oven, it is dry under conditions of temperature is 50~60 DEG C and vacuum degree is 80~100Pa
10~12h obtains drying composite, and the sulfuric acid solution investment that desciccate, graphite flake and mass fraction are 30~40% is placed in
It is uniformly mixed and is made to reaction solution in the beaker of ice-water bath, potassium permanganate powder is added into three-necked flask, with blender with 200
The revolving speed of~240r/min is mixed 50~60min and oxidation liquid is made；
The specific preparation step of the mixed solution are as follows:
(1) sawdust and agricultural crop straw are put into baking oven, dry 5~6h under conditions of temperature is 70~80 DEG C, after dry
It puts into planetary ball mill, 2~3h is ground under conditions of ratio of grinding media to material is 10:1 and revolving speed is 150~180r/min, is ground
Mixture is ground, the hydrochloric acid that milled mixtures and mass fraction are 4~8% is put into beaker, with agitating device with 300~400r/
45~60min is mixed under conditions of min, mixed serum is made；
(2) mixed serum is put into reaction kettle, nitrogen is filled with into reaction kettle until in reaction kettle air pressure be increased to 1.6~
2.0MPa increases reactor temperature to 160~180 DEG C, and mass fraction is added dropwise thereto and is by 60~80min of constant temperature and pressure reaction
3~6% sodium bicarbonate solution adjusts pH value to neutrality, reaction hydrolyzate is made, by reaction hydrolyzate and methane liquid investment fermentation
In tank；
(3) fermentor is sealed, is placed in the greenhouse that ambient temperature is 32~36 DEG C, constant temperature stands 5~7 days, obtains after standing
Tunning is placed in microwave equipment by tunning, in lift apparatus temperature to 120~140 DEG C, constant temperature stands 30~
Microwave reaction liquid is made in 40min, will be uniformly mixed to obtain mixed solution in microwave reaction liquid and Aluminium Sulphate usp (powder) investment beaker.
2. a kind of preparation method of high viscosity high intensity raw lacquer according to claim 1, it is characterised in that: preferred by weight
Number meter is measured, the filter cake is 8~10 parts, raw lacquer liquid is 23~25 parts, manganese naphthenate is 1.0~1.2 parts, ethylene glycol 2
~3 parts.
3. a kind of preparation method of high viscosity high intensity raw lacquer according to claim 1, it is characterised in that: preferred by weight
Number meter is measured, the prefabricated mixed liquor is 35~37 parts, SiO 2 powder is 1~3 part, silane coupling agent is 2~4 parts,
The acetum that mass fraction is 4~8% is 4~6 parts.
4. a kind of preparation method of high viscosity high intensity raw lacquer according to claim 1, it is characterised in that: oxidation liquid
Specific preparation step (2) in it is preferred according to parts by weight, the desciccate is 6~8 parts, graphite flake is 2~3 parts,
The sulfuric acid solution that mass fraction is 30~40% is 12~16 parts.
5. a kind of preparation method of high viscosity high intensity raw lacquer according to claim 1, it is characterised in that: oxidation liquid
Specific preparation step (2) described in the quality of potassium permanganate powder that is added into three-necked flask be to reaction solution quality
4~6%.
6. a kind of preparation method of high viscosity high intensity raw lacquer according to claim 1, it is characterised in that: mixed solution
The mass ratio of sawdust described in specific preparation step (1) and agricultural crop straw is 3:1.
7. a kind of preparation method of high viscosity high intensity raw lacquer according to claim 1, it is characterised in that: mixed solution
The mass ratio for the hydrochloric acid that milled mixtures and mass fraction described in specific preparation step (1) are 4~8% is 1:10.
8. a kind of preparation method of high viscosity high intensity raw lacquer according to claim 1, it is characterised in that: mixed solution
The mass ratio of reaction hydrolyzate described in specific preparation step (2) and methane liquid is 15:1.
9. a kind of preparation method of high viscosity high intensity raw lacquer according to claim 1, it is characterised in that: mixed solution
The mass ratio of microwave reaction liquid described in specific preparation step (3) and Aluminium Sulphate usp (powder) is 15:1.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111647355A (en) * | 2020-07-17 | 2020-09-11 | 利川市德隆生漆科技有限责任公司 | Natural raw lacquer coating special for ancient building repair and manufacturing and blending method thereof |
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| CN107955532A (en) * | 2017-12-25 | 2018-04-24 | 中山市得高行知识产权中心（有限合伙） | A kind of lignose raw lacquer composite coating |
| CN107987661A (en) * | 2017-12-29 | 2018-05-04 | 西北农林科技大学 | A kind of biomass graphene modified raw lacquer heavy antisepsis composite coating and preparation method thereof |
| CN108997935A (en) * | 2018-05-25 | 2018-12-14 | 繁昌县若木营造装饰工程有限公司 | A kind of modified raw lacquer composite coating and preparation method thereof |
| CN109135377A (en) * | 2018-09-21 | 2019-01-04 | 佛山齐安建筑科技有限公司 | A kind of preparation method of curing compound |
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| US20160237194A1 (en) * | 2013-09-30 | 2016-08-18 | Upm-Kymmene Corporation | A method for increasing the reactivity of lignin |
| CN105779528A (en) * | 2014-12-22 | 2016-07-20 | 中国石油化工股份有限公司 | Lignocellulose continuous enzymatic hydrolysis and synchronous saccharification-fermentation method |
| CN107955532A (en) * | 2017-12-25 | 2018-04-24 | 中山市得高行知识产权中心（有限合伙） | A kind of lignose raw lacquer composite coating |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111647355A (en) * | 2020-07-17 | 2020-09-11 | 利川市德隆生漆科技有限责任公司 | Natural raw lacquer coating special for ancient building repair and manufacturing and blending method thereof |
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Application publication date: 20190705 |