CN109337437A - A kind of preparation process of solubility environment-friendly ink - Google Patents
A kind of preparation process of solubility environment-friendly ink Download PDFInfo
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- CN109337437A CN109337437A CN201811191602.4A CN201811191602A CN109337437A CN 109337437 A CN109337437 A CN 109337437A CN 201811191602 A CN201811191602 A CN 201811191602A CN 109337437 A CN109337437 A CN 109337437A
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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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
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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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
- C09D11/037—Printing inks characterised by features other than the chemical nature of the binder characterised by the pigment
Abstract
The invention discloses a kind of preparation process of soluble environment-friendly ink, specific preparation process is as follows: a certain amount of fluorinated polyimide binding material being added in acetone soln, stirring and dissolving；Distributed pigment is added in solution into the first step, high-speed stirred mixes 3-5min, and varnish, dispersing agent, defoaming agent, wetting agent are then added thereto, is uniformly mixed under room temperature and obtains soluble environment-friendly ink.The present invention uses the fluorinated polyimide binding material of preparation as ink binder, not only adhesive force with higher, it being capable of firm adhesion ink, the distributed surface of pigments in ink contains one layer of hydrophobic membrane simultaneously, it can ensure the hydrophobic water-resistant capacity of ink, so that ink will not be removed in water, simultaneously using fluorinated polyimide as binding material, acetone can be quickly dissolved in, pyridine, in the sulfuric acid solution that tetrahydrofuran and concentration are 2%, so that pigment does not have the effect of bonding force to be directly dissolved in solvent, and then realize the removing of billboard surface spraying trace.
Description
Technical field
The invention belongs to field of ink preparation, are related to a kind of preparation process of soluble environment-friendly ink.
Background technique
Ink is to be closed auxiliary agent by pigment, link stuff and be mixed with according to a certain percentage, may be implemented to print by ink
Label meets the needs of people's record, and existing billboard passes through post ads paper mostly, convenient for the replacement of billboard, still
When replacing poster paper, discarded poster paper, which directly abandons, be easy to cause waste, while existing billboard typically directly will be oily
Ink print is on poster paper, in extraneous exposing to the weather, corrodes to be easy to fade in printed mark in the long-time of rainwater and even peel off.
Summary of the invention
It is sub- using the fluorination polyamides of preparation the purpose of the present invention is to provide a kind of preparation process of soluble environment-friendly ink
Amine binding material is as ink binder, not only adhesive force with higher, can firm adhesion ink, while in ink
Distributed surface of pigments contains one layer of hydrophobic membrane, can ensure the hydrophobic water-resistant capacity of ink, so that ink will not be shelled in water
From, while using fluorinated polyimide as binding material, can quickly be dissolved in acetone, pyridine, tetrahydrofuran and concentration is 2%
Sulfuric acid solution in so that pigment does not have the effect of bonding force to be directly dissolved in solvent, and then realize the spraying of billboard surface
The removing of trace, and ink trace is absolutely not left after removing, and then be convenient for the recycling of billboard, solve existing advertisement
Board passes through post ads paper mostly, and convenient for the replacement of billboard, but when replacing poster paper, discarded poster paper is directly abandoned
The problem of be easy to causeing waste.
Fluorinated polyimide binding material prepared by the present invention is 2% being soaked in acetone, pyridine, tetrahydrofuran and concentration
After in sulfuric acid solution, the 5-6 dissolution that ink trace can be realized is brushed at mark using hairbrush, is handled quick and convenient.
Fluorinated polyimide binding material adhesive force with higher prepared by the present invention, so that printing trace is grown in water
Time remains to bonding securely when impregnating, do not remove, and then be able to solve existing billboard and be typically directly printed on ink extensively
It accuses on paper, in extraneous exposing to the weather, is corroded the problem of printed mark is easy to fade even peeling in the long-time of rainwater.
Contain a large amount of fluorine atom in fluorinated polyimide binding material molecular structure prepared by the present invention, since fluorine atom can
To cut off the conjugation of electron cloud in acid imide molecule, destroys the structural symmetry of acid imide molecule and repeat regularity, poly-
Contain fluorine atom between each monomer molecule during conjunction, so that on the fluorinated polyimide binding material overall molecule chain of preparation
Structural symmetry and repeat regularity destroyed, thereby reduce the active force and crystallinity of rigid olyurethane strand,
And then improve the solvability of fluorinated polyimide binding material, while calcium chloride being added during the reaction, calcium therein from
Son forms complex compound with binding material and further improves the solvability of binding material, makes it in acetone, pyridine, tetrahydrofuran and dense
It can quickly be dissolved in the sulfuric acid solution that degree is 2%.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of preparation process of solubility environment-friendly ink, specific preparation process are as follows:
The first step a certain amount of fluorinated polyimide binding material is added in acetone soln, stirring and dissolving；
Distributed pigment is added in the solution into the first step for second step, and high-speed stirred mixes 3-5min, then thereto
Varnish, dispersing agent, defoaming agent, wetting agent is added, is uniformly mixed under room temperature and obtains soluble environment-friendly ink；
Wherein the parts by weight of each component are as follows in soluble environment-friendly ink:
52-55 parts of fluorinated polyimide binding material, distributed 46-48 parts of pigment, 5-7 parts of varnish, 1-2 parts of dispersing agent,
1-2 parts of defoaming agent, 2-3 parts of wetting agent, 100 parts of acetone；
The specific preparation process of distributed pigment is as follows:
1. a certain amount of ethylenediamine is soluble in water, while pigment being added thereto, it is uniformly mixed；
2. to step 1. in γ-glycidyl ether oxygen propyl trimethoxy silicane is added dropwise, while be added dropwise while be vigorously stirred,
Isothermal reaction 40-50min, is then filtered washing, obtains distributed pigment after being added dropwise completely；Since ethylenediamine is dissolved in water,
It can be dispersed in around surface of pigments, while γ-glycidyl ether oxygen propyl trimethoxy silicane is not soluble in water, therefore straight
It connects and is reacted on the surface of pigment with ethylenediamine, so that the surface of pigment forms one layer of composite membrane, due to γ-glycidol ether
Contain alkoxy in oxygen propyl trimethoxy silicane, therefore composite membrane is with higher hydrophobic and dispersibility, is preparing ink
It can be uniformly dispersed in solution during a, reaction structure formula is as follows；Ethylenediamine 0.75- is wherein added in every gram of pigment
γ-glycidyl ether oxygen propyl trimethoxy silicane 0.83-0.85g is added in 0.78g；
Wherein the specific preparation process of fluorinated polyimide binding material is as follows:
Step 1: it takes a certain amount of aniline and p-trifluoromethyl benzaldehyde to be added to the water, while concentrated hydrochloric acid being added thereto,
It is warming up to 150-160 DEG C of back flow reaction 12h, rotary evaporation is then carried out and removes the wherein complete raw material of unreacted, then carry out
It is recrystallized to give fluorinated diamine monomer, reaction structure formula is as shown in Figure 1；P-trifluoromethyl benzaldehyde wherein is added in every gram of aniline
1.93-1.96g concentrated hydrochloric acid 0.03g is added；
Step 2: after being passed through nitrogen 10min into reaction vessel, by a certain amount of fluorinated diamine monomer and trimellitic anhydride
It is added in reaction vessel, n,N-Dimethylformamide is then added thereto again, is warming up to 100 DEG C of reaction 5h, is then cooled to
Fixed particle is precipitated after room temperature and is filtered washing, obtains product A；Amino there are two wherein containing in fluorinated diamine monomer, can
Open loop substitution reaction occurs with the anhydride group of trimellitic anhydride, so that trimellitic anhydride is compounded in the two of fluorinated diamine monomer
Side, so that trifluoromethyl is in the middle position on product A chain in the product A of preparation, reaction structure formula is as follows；Wherein every gram of fluorine
Change and trimellitic anhydride 0.56-0.57g is added in diamine monomer, N,N-dimethylformamide 6-8mL is added；
Step 3: the product A prepared in step 2 being added in pyridine, is then added under nitrogen protection into reaction vessel
Acetic anhydride is warming up to 100 DEG C of reaction 4h, is then filtered washing and obtains fluorinated imide, due to trifluoro in fluorinated imide
Methyl is in the middle position on fluorinated imide chain, and it is electronegativity, lesser atomic radius and lower that fluorine atom, which has larger,
Mole polarizability, allow fluorine atom to cut off the conjugation of electron cloud in acid imide molecule, destroy the knot of acid imide molecule
Structure symmetry and repetition regularity, wherein reaction structure formula is as follows: pyridine 9-11mL being added in every gram of product A, acetic anhydride is added
0.82-0.85g；
Step 4: weighing a certain amount of fluorinated diamine monomer and be dissolved in dimethyl sulfoxide, nitrogen is passed through into reaction vessel
Then fluorinated imide, calcium chloride and triphenyl phosphite is added in 10min, then heat to 120 DEG C of reaction 5h, product cooling
Filtration washing is carried out after to room temperature, obtains fluorinated polyimide binding material, since fluorine atom can cut off electricity in acid imide molecule
The conjugation of sub- cloud destroys the structural symmetry of acid imide molecule and repeats regularity, in the course of the polymerization process each monomer molecule
Between contain fluorine atom so that preparation fluorinated polyimide binding material overall molecule chain on structural symmetry and repeat advise
Whole property is destroyed, and the active force and crystallinity of rigid olyurethane strand are thereby reduced, and then it is sub- to improve fluorination polyamides
The solvability of amine binding material, while calcium chloride being added during the reaction, calcium ion therein and binding material form complex compound
The solvability of binding material is further improved, reaction structure formula is as follows；Dimethyl wherein is added in every gram of fluorinated diamine monomer
Fluorinated imide 2.35-2.41g is added in sulfoxide 7mL, and calcium chloride 0.83-0.86g is added, and triphenyl phosphite 0.2g is added；
The dissolution process process of the solubility environment-friendly ink is as follows: being brushed and is marked in plastic sheet surface with soluble environment-friendly ink
Plastic plate is separately immersed in the sulfuric acid solution that acetone, pyridine, tetrahydrofuran and concentration are 2% by will after mark dries,
It is brushed at the mark of plastic sheet surface using hairbrush, the ink of plastic sheet surface is quickly dissolved into solvent, plastic sheet surface
Ink trace is not left, since the pigment in ink is adhesively fixed by binding material, when binding material is soluble in acetone, face
Material is directly removed from plastic sheet surface under the action of no cohesive force, and then realizes soluble environment-friendly ink in a solvent molten
Solution.
Beneficial effects of the present invention:
The present invention uses the fluorinated polyimide binding material of preparation as ink binder, not only bonding energy with higher
Power, can firm adhesion ink, while the distributed surface of pigments in ink contains one layer of hydrophobic membrane, can ensure ink
Hydrophobic water-resistant capacity, so that ink will not be removed in water, while using fluorinated polyimide as binding material, it can be quickly molten
Solution is in the sulfuric acid solution that acetone, pyridine, tetrahydrofuran and concentration are 2%, so that pigment does not have the effect of bonding force directly molten
Solution in a solvent, and then realizes the removing of billboard surface spraying trace, and absolutely not leave ink trace, Jin Erbian after removing
In the recycling of billboard, solves existing billboard and pass through post ads paper mostly, convenient for the replacement of billboard, but
When replacing poster paper, discarded poster paper directly abandons the problem of be easy to causeing waste.
Fluorinated polyimide binding material prepared by the present invention is 2% being soaked in acetone, pyridine, tetrahydrofuran and concentration
After in sulfuric acid solution, the 5-6 dissolution that ink trace can be realized is brushed at mark using hairbrush, is handled quick and convenient.
Fluorinated polyimide binding material adhesive force with higher prepared by the present invention, so that printing trace is grown in water
Time remains to bonding securely when impregnating, do not remove, and then be able to solve existing billboard and be typically directly printed on ink extensively
It accuses on paper, in extraneous exposing to the weather, is corroded the problem of printed mark is easy to fade even peeling in the long-time of rainwater.
Contain a large amount of fluorine atom in fluorinated polyimide binding material molecular structure prepared by the present invention, since fluorine atom can
To cut off the conjugation of electron cloud in acid imide molecule, destroys the structural symmetry of acid imide molecule and repeat regularity, poly-
Contain fluorine atom between each monomer molecule during conjunction, so that on the fluorinated polyimide binding material overall molecule chain of preparation
Structural symmetry and repeat regularity destroyed, thereby reduce the active force and crystallinity of rigid olyurethane strand,
And then improve the solvability of fluorinated polyimide binding material, while calcium chloride being added during the reaction, calcium therein from
Son forms complex compound with binding material and further improves the solvability of binding material, makes it in acetone, pyridine, tetrahydrofuran and dense
It can quickly be dissolved in the sulfuric acid solution that degree is 2%.
Detailed description of the invention
In order to facilitate the understanding of those skilled in the art, the present invention will be further described below with reference to the drawings.
Fig. 1 is the distributed pigment reaction structure formula of the present invention；
Fig. 2 is fluorinated diamine monomer reaction structural formula of the present invention；
Fig. 3 is fluorinated imide reaction structure formula；
Fig. 4 is fluorinated polyimide binding material reaction structure formula.
Specific embodiment
Fig. 1-4 is please referred to, is described in detail in conjunction with following examples:
Embodiment 1:
The specific preparation process of distributed pigment is as follows:
1. 750g ethylenediamine is soluble in water, while 1kg pigment being added thereto, it is uniformly mixed；
2. to step 1. in 830g γ-glycidyl ether oxygen propyl trimethoxy silicane is added dropwise, while be added dropwise while it is violent
Stirring, isothermal reaction 40-50min, is then filtered washing, obtains distributed pigment after being added dropwise completely；
The specific preparation process of fluorinated polyimide binding material is as follows:
Step 1: taking 1kg aniline and 1.93kg p-trifluoromethyl benzaldehyde to be added in 1L water, while it is dense that 30g is added thereto
Then hydrochloric acid, temperature carry out rotary evaporation and remove the wherein complete raw material of unreacted to 150-160 DEG C of back flow reaction 12h, then into
Row is recrystallized to give fluorinated diamine monomer；
Step 2: after being passed through nitrogen 10min into reaction vessel, 1kg fluorinated diamine monomer and 560g trimellitic anhydride being added
Enter in reaction vessel, 6LN is then added thereto again, dinethylformamide is warming up to 100 DEG C of reaction 5h, is then cooled to
Fixed particle is precipitated after room temperature and is filtered washing, obtains product A；
Step 3: the 1kg product A prepared in step 2 being added in 9L pyridine, then under nitrogen protection to reaction vessel
Middle addition 820g acetic anhydride is warming up to 100 DEG C of reaction 4h, is then filtered washing and obtains fluorinated imide；
Step 4: weighing 1kg fluorinated diamine monomer and be dissolved in 7L dimethyl sulfoxide, nitrogen is passed through into reaction vessel
Then 2.35kg fluorinated imide, 830g calcium chloride and 200g triphenyl phosphite is added in 10min, then heat to 120 DEG C instead
Filtration washing is carried out after answering 5h, product to be cooled to room temperature, obtains fluorinated polyimide binding material.
Embodiment 2:
The specific preparation process of distributed pigment is as follows:
1. 780g ethylenediamine is soluble in water, while 1kg pigment being added thereto, it is uniformly mixed；
2. to step 1. in 850g γ-glycidyl ether oxygen propyl trimethoxy silicane is added dropwise, while be added dropwise while it is violent
Stirring, isothermal reaction 40-50min, is then filtered washing, obtains distributed pigment after being added dropwise completely；
The specific preparation process of fluorinated polyimide binding material is as follows:
Step 1: taking 1kg aniline and 1.96kg p-trifluoromethyl benzaldehyde to be added in 1L water, while it is dense that 30g is added thereto
Then hydrochloric acid, temperature carry out rotary evaporation and remove the wherein complete raw material of unreacted to 150-160 DEG C of back flow reaction 12h, then into
Row is recrystallized to give fluorinated diamine monomer；
Step 2: after being passed through nitrogen 10min into reaction vessel, 1kg fluorinated diamine monomer and 570g trimellitic anhydride being added
Enter in reaction vessel, 8LN is then added thereto again, dinethylformamide is warming up to 100 DEG C of reaction 5h, is then cooled to
Fixed particle is precipitated after room temperature and is filtered washing, obtains product A；
Step 3: the 1kg product A prepared in step 2 being added in 11L pyridine, then under nitrogen protection to reaction vessel
Middle addition 850g acetic anhydride is warming up to 100 DEG C of reaction 4h, is then filtered washing and obtains fluorinated imide；
Step 4: weighing 1kg fluorinated diamine monomer and be dissolved in 7L dimethyl sulfoxide, nitrogen is passed through into reaction vessel
Then 2.41kg fluorinated imide, 860g calcium chloride and 200g triphenyl phosphite is added in 10min, then heat to 120 DEG C instead
Filtration washing is carried out after answering 5h, product to be cooled to room temperature, obtains fluorinated polyimide binding material.
Embodiment 3:
A kind of preparation process of solubility environment-friendly ink, specific preparation process are as follows:
The first step, fluorinated polyimide binding material prepared by 5.2kg embodiment 1 are added in 10kg acetone soln, stirring
Dissolution；
Second step, distributed pigment prepared by 4.6kg embodiment 1 is added in the solution into the first step, and high-speed stirred is mixed
3-5min is closed, 0.5kg varnish, 0.1kg dispersing agent, 0.1kg defoaming agent, 0.2kg wetting agent are then added thereto, under room temperature
It is uniformly mixed and obtains soluble environment-friendly ink.
Embodiment 4:
A kind of preparation process of solubility environment-friendly ink, specific preparation process are as follows:
The first step, fluorinated polyimide binding material prepared by 5.5kg embodiment 2 are added in 10kg acetone soln, stirring
Dissolution；
Second step, distributed pigment prepared by 4.8kg embodiment 2 is added in the solution into the first step, and high-speed stirred is mixed
3-5min is closed, 0.7kg varnish, 0.2kg dispersing agent, 0.2kg defoaming agent, 0.3kg wetting agent are then added thereto, under room temperature
It is uniformly mixed and obtains soluble environment-friendly ink.
Embodiment 5:
A kind of preparation process of solubility environment-friendly ink, specific preparation process are as follows:
The first step, fluorinated polyimide binding material prepared by 5.2kg embodiment 1 are added in 10kg acetone soln, stirring
Dissolution；
4.6kg pigment is added in the solution into the first step for second step, and high-speed stirred mixes 3-5min, then thereto
0.5kg varnish, 0.1kg dispersing agent, 0.1kg defoaming agent, 0.2kg wetting agent is added, is uniformly mixed under room temperature and obtains solubility
Environment-friendly ink.
Embodiment 6:
A kind of preparation process of solubility environment-friendly ink, specific preparation process are as follows:
The first step 5.2kg polyurethane binder is added in 10kg acetone soln, stirring and dissolving；
Second step, distributed pigment prepared by 4.6kg embodiment 1 is added in the solution into the first step, and high-speed stirred is mixed
3-5min is closed, 0.5kg varnish, 0.1kg dispersing agent, 0.1kg defoaming agent, 0.2kg wetting agent are then added thereto, under room temperature
It is uniformly mixed and obtains soluble environment-friendly ink.
Embodiment 7:
A kind of preparation process of solubility environment-friendly ink, specific preparation process are as follows:
The first step 5.2kg epobond epoxyn is added in 10kg acetone soln, stirring and dissolving；
Second step, distributed pigment prepared by 4.6kg embodiment 1 is added in the solution into the first step, and high-speed stirred is mixed
3-5min is closed, 0.5kg varnish, 0.1kg dispersing agent, 0.1kg defoaming agent, 0.2kg wetting agent are then added thereto, under room temperature
It is uniformly mixed and obtains soluble environment-friendly ink.
Embodiment 8:
A kind of preparation process of solubility environment-friendly ink, specific preparation process are as follows:
The first step 5.2kg aerodux is added in 10kg acetone soln, stirring and dissolving；
Second step, distributed pigment prepared by 4.6kg embodiment 1 is added in the solution into the first step, and high-speed stirred is mixed
3-5min is closed, 0.5kg varnish, 0.1kg dispersing agent, 0.1kg defoaming agent, 0.2kg wetting agent are then added thereto, under room temperature
It is uniformly mixed and obtains soluble environment-friendly ink.
Embodiment 9
Dissolution process after brushing to the soluble environment-friendly ink of embodiment 3-8 preparation, concrete processing procedure are as follows: using
Soluble environment-friendly ink is brushed in plastic sheet surface to be indicated, after mark dries, plastic plate is separately immersed in acetone, water, pyrrole
Pyridine, tetrahydrofuran, ethanol solution, concentration be 2% sulfuric acid solution in, brush 5- at the mark of plastic sheet surface using hairbrush
6 times, the results are shown in Table 1；
The dissolution situation of the soluble environment-friendly ink printing plastic plate ink in different solvents of table 1
As shown in Table 1, use the fluorinated polyimide binding material of preparation as ink binder, it is not only with higher viscous
Conjunction ability, can firm adhesion ink, while the distributed surface of pigments in ink contains one layer of hydrophobic membrane, can ensure oil
The hydrophobic water-resistant capacity of ink, so that ink will not be removed in water, while using fluorinated polyimide as binding material, it can be quick
Be dissolved in acetone, pyridine, tetrahydrofuran and concentration be 2% sulfuric acid solution in so that pigment does not have the effect of bonding force straight
It connects dissolution in a solvent, and then realizes the removing of plastic sheet surface spraying trace, and absolutely not leave ink trace after removing.
Embodiment 10
The soluble environment-friendly ink of embodiment 3-8 preparation is brushed in plastic sheet surface and is indicated, after mark dries, will be moulded
The case where flitch observes printed mark after impregnating in water 10 days, 30 days, 50 days, the results are shown in Table 2；
Table 2: dissolubility environment-friendly ink brushes the situation after mark impregnates different time in water in plastic sheet surface
As shown in Table 2, fluorinated polyimide is as binding material, adhesive force with higher, so that printing trace is in water
Middle long-time remains to bonding securely when impregnating, do not remove.
Present invention disclosed above preferred embodiment is only intended to help to illustrate the present invention.There is no detailed for preferred embodiment
All details are described, are not limited the invention to the specific embodiments described.Obviously, according to the content of this specification,
It can make many modifications and variations.These embodiments are chosen and specifically described to this specification, is in order to better explain the present invention
Principle and practical application, so that skilled artisan be enable to better understand and utilize the present invention.The present invention is only
It is limited by claims and its full scope and equivalent.
Claims (10)
1. a kind of preparation process of solubility environment-friendly ink, which is characterized in that specific preparation process is as follows:
The first step a certain amount of fluorinated polyimide binding material is added in acetone soln, stirring and dissolving；
Second step, distributed pigment is added in the solution into the first step, and high-speed stirred mixes 3-5min, is then added thereto
Varnish, dispersing agent, defoaming agent, wetting agent are uniformly mixed under room temperature and obtain soluble environment-friendly ink；
Wherein the specific preparation process of fluorinated polyimide binding material is as follows:
Step 1: taking a certain amount of aniline and p-trifluoromethyl benzaldehyde to be added to the water, while concentrated hydrochloric acid being added thereto, heat up
To 150-160 DEG C of back flow reaction 12h, then carries out rotary evaporation and remove the wherein complete raw material of unreacted, then tied again
Crystalline substance obtains fluorinated diamine monomer；
Step 2: after being passed through nitrogen 10min into reaction vessel, a certain amount of fluorinated diamine monomer and trimellitic anhydride being added
In reaction vessel, n,N-Dimethylformamide is then added thereto again, is warming up to 100 DEG C of reaction 5h, is then cooled to room temperature
Fixed particle is precipitated afterwards and is filtered washing, obtains product A；
Step 3: the product A prepared in step 2 being added in pyridine, acetic acid is then added into reaction vessel under nitrogen protection
Acid anhydride is warming up to 100 DEG C of reaction 4h, is then filtered washing and obtains fluorinated imide；
Step 4: it weighs a certain amount of fluorinated diamine monomer and is dissolved in dimethyl sulfoxide, nitrogen 10min is passed through into reaction vessel,
Then fluorinated imide, calcium chloride and triphenyl phosphite is added, then heats to 120 DEG C of reaction 5h, product is cooled to room temperature
After carry out filtration washing, obtain fluorinated polyimide binding material.
2. a kind of preparation process of soluble environment-friendly ink according to claim 1, which is characterized in that soluble environment protection oil
The parts by weight of each component are as follows in ink: 52-55 parts of fluorinated polyimide binding material, distributed 46-48 parts of pigment, varnish 5-7
Part, 1-2 parts of dispersing agent, 1-2 parts of defoaming agent, 2-3 parts of wetting agent, 100 parts of acetone.
3. a kind of preparation process of soluble environment-friendly ink according to claim 1, which is characterized in that in step 1, every gram
P-trifluoromethyl benzaldehyde 1.93-1.96g is added in aniline, concentrated hydrochloric acid 0.03g is added.
4. a kind of preparation process of soluble environment-friendly ink according to claim 1, which is characterized in that every gram in step 2
Trimellitic anhydride 0.56-0.57g is added in fluorinated diamine monomer, N,N-dimethylformamide 6-8mL is added.
5. a kind of preparation process of soluble environment-friendly ink according to claim 1, which is characterized in that every gram in step 3
Pyridine 9-11mL is added in product A, acetic anhydride 0.82-0.85g is added.
6. a kind of preparation process of soluble environment-friendly ink according to claim 1, which is characterized in that every gram in step 4
Dimethyl sulfoxide 7mL is added in fluorinated diamine monomer, fluorinated imide 2.35-2.41g is added, calcium chloride 0.83- is added
Triphenyl phosphite 0.2g is added in 0.86g.
7. a kind of preparation process of soluble environment-friendly ink according to claim 1, which is characterized in that distributed pigment
Specific preparation process is as follows:
1. a certain amount of ethylenediamine is soluble in water, while pigment being added thereto, it is uniformly mixed；
2. to step 1. in γ-glycidyl ether oxygen propyl trimethoxy silicane is added dropwise, while be added dropwise while be vigorously stirred, be added dropwise
Isothermal reaction 40-50min, is then filtered washing, obtains distributed pigment after completely.
8. a kind of preparation process of soluble environment-friendly ink according to claim 7, which is characterized in that add in every gram of pigment
Enter ethylenediamine 0.75-0.78g, γ-glycidyl ether oxygen propyl trimethoxy silicane 0.83-0.85g is added.
9. a kind of preparation process of soluble environment-friendly ink according to claim 1, which is characterized in that solubility environmental protection
The dissolution process process of ink is as follows: being brushed and is indicated in plastic sheet surface with soluble environment-friendly ink, after mark dries, will moulded
Flitch impregnates in a solvent, is brushed at the mark of plastic sheet surface using hairbrush, the ink of plastic sheet surface is quickly dissolved into
In solvent, plastic sheet surface does not leave ink trace.
10. a kind of preparation process of soluble environment-friendly ink according to claim 9, which is characterized in that the solvent is
One of the sulfuric acid solution that acetone, pyridine, tetrahydrofuran or concentration are 2%.
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| CN114729215A (en) * | 2020-10-20 | 2022-07-08 | 律胜科技股份有限公司 | Curable composition for inkjet, cured product, and flexible printed wiring board |
Citations (7)
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| CN104592809A (en) * | 2015-02-04 | 2015-05-06 | 韦棋 | High-adhesive force printing ink |
| CN106661244A (en) * | 2014-07-03 | 2017-05-10 | 大金工业株式会社 | Film |
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| CN1639262A (en) * | 2002-01-15 | 2005-07-13 | 株式会社Pi技术研究所 | Solvent-soluble block copolyimide composition and process for producing the same |
| CN1965039A (en) * | 2004-05-27 | 2007-05-16 | 株式会社Pi技术研究所 | Block copolymerized polyimide ink composition for printing |
| CN102504255A (en) * | 2011-11-01 | 2012-06-20 | 东南大学 | Soluble fluorinated polyimide material and preparation method thereof |
| CN102585607A (en) * | 2012-03-28 | 2012-07-18 | 成都多吉昌新材料有限公司 | Solder mask ink composite and method for manufacturing solder mask layer of light-emitting diode (LED) circuit board |
| CN103897489A (en) * | 2012-12-31 | 2014-07-02 | 中原工学院 | Fluoridated polyimide-base ink-jet printer ink for solar cells and preparation method thereof |
| CN106661244A (en) * | 2014-07-03 | 2017-05-10 | 大金工业株式会社 | Film |
| CN104592809A (en) * | 2015-02-04 | 2015-05-06 | 韦棋 | High-adhesive force printing ink |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114729215A (en) * | 2020-10-20 | 2022-07-08 | 律胜科技股份有限公司 | Curable composition for inkjet, cured product, and flexible printed wiring board |
| CN114729215B (en) * | 2020-10-20 | 2023-11-10 | 律胜科技股份有限公司 | Curable composition for inkjet, cured product, and flexible printed circuit board |
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