CN102732055A - Multi-component chromogenic anion co-intercalation supramolecular structure pigment and preparation method thereof - Google Patents
Multi-component chromogenic anion co-intercalation supramolecular structure pigment and preparation method thereof Download PDFInfo
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Abstract
The invention provides a multi-component chromogenic anion co-intercalation supramolecular structure pigment and a preparation method thereof. The multi-component chromogenic anion co-intercalation supramolecular structure pigment has a general chemical formula of M<2+>1-xM<3+>x(OH)2(A<n->)x/n.mH2O. The preparation method comprises the following steps of mixing a mixed salt solution, a mixed solution of two or more chromogenic anionic compounds, and an alkali solution, and simultaneously inserting chromogenic anions between hydrotalcite layers so that a series of the multi-component chromogenic anion co-intercalation supramolecular structure pigment is prepared. A color of the multi-component chromogenic anion co-intercalation supramolecular structure pigment is different from that of a single-component chromogenic anion co-intercalation supramolecular structure pigment and can be adjusted through adjustment of a mole ratio of different chromogenic anions inserted between hydrotalcite layers. The preparation method is simple and is convenient for large scale production.
Description
Affiliated field
The present invention relates to a kind of polycomponent colour developing negatively charged ion intercalation supramolecular structure pigment and preparation method thereof altogether.
Background technology
Hydrotalcite (Layered Double Hydroxides; Be abbreviated as LDHs) be a kind of anionic type laminated material; Because but it has the performance of intercalation assembling; Thereby utilize this performance can some function negatively charged ion be inserted into hydrotalcite layers, prepare supermolecular intercalation structure material with specific function.
Document Rafael Marangoni, Christine Taviot-Gu é ho, Abdallah Illaik; Fernando Wypych, FabriceLeroux, Journal of Colloid and Interface Science; 2008,366-373 adopts coprecipitation method will contain Zn
2+And Al
3+Mixing salt solution and NaOH alkaline solution be added drop-wise in the dye solution simultaneously; The pH=9 of adjustment reaction system; Obtain interlayer and be respectively sun blue 1, sun blue 53 and the anionic intercalated houghite of Niagara blue, with the intercalation product as fillers dispersed in PS; Investigated filler p-poly-phenyl ethene second-order transition temperature, the influence of rheological property and optical property.
Document Umberto Costanino, Natascia Coletti, and Morena Nocchetti, Langmuir, 1999, among the 15:4454-4460, adopt the urea thermal synthesis method to obtain hydrotalcite [Zn earlier
0.67Al
0.33(OH)
2] [CO
3]
0.1650.4H
2O obtains hydrotalcite Zn with itself and NaCl and HCl reaction again
0.67Al
0.33(OH)
2Cl
0.330.4H
2O is again with Zn
0.67Al
0.33(OH)
2Cl
0.330.4H
2O is a precursor, and tropeolin-D (MO) is object, and assembling obtains intercalated houghite [Zn
0.67Al
0.33(OH)
2] [MO
0.31Cl
0.02] 0.85H
2O, they have investigated the fluorescence of product.
Above document just is inserted into hydrotalcite layers with a kind of dyestuff negatively charged ion, can only prepare a kind of pigment of color.Because can producing when mixing, different colour developing negatively charged ion are different from the anionic new color of original colour developing; Thereby the colour developing negatively charged ion of two or more different colours is inserted into hydrotalcite layers simultaneously, then can prepare color and be different from the anion intercalated supramolecular structure pigment of single colour developing.
Summary of the invention
The purpose of this invention is to provide a kind of polycomponent colour developing negatively charged ion and be total to supramolecular structure pigment of intercalation and preparation method thereof.Colour developing negatively charged ion through with two or more different colours is inserted into hydrotalcite layers simultaneously; And can regulate and control the color of prepared pigment, thereby prepare a series of polycomponents colour developing negatively charged ion supramolecular structure pigment of intercalation altogether through the negatively charged ion ratio that modulation inserts hydrotalcite layers.
The chemical general formula of the supermolecular intercalation structure pigment of the present invention's preparation is:
M
2+ 1-xM
3+ x(OH)
2(A
n-)
x/n·mH
2O
0.1≤x≤0.5 wherein, m is an interlayer crystal water molecule number; M
2+Be divalent-metal ion Mg
2+, Zn
2+, Ni
2+, Ca
2+, Fe
2+Or Cu
2+In any one or two kinds, preferably Mg
2+Or Zn
2+M
3+Be trivalent metal ion Al
3+, Co
3+, Ti
3+, Fe
3+Or Cr
3+In any one or two kinds, preferably Al
3+A
N-Be two or more colour developing negatively charged ion;
The colour developing anionic compound that can be used for intercalation divides dyestuff and pigment dyestuff precursor two big classes, and wherein dyestuff has matching stain, mordant dyes, reactive dyestuffs, substantive dyestuff; The pigment dyestuff precursor is the sodium salt or the acid precursor of pigment dyestuff.
Described matching stain has turmeric yellow, Xylene Red, von Muller's indicator, acid green, acid blue; Wherein acid yellow dye has quinoline yellow, acid yellow 11, turmeric yellow 13, turmeric yellow 14, turmeric yellow 17, turmeric yellow 19, turmeric yellow 25, quinoline yellow 6, quinoline yellow 8, turmeric yellow 40, turmeric yellow 42, turmeric yellow 44, turmeric yellow 49, turmeric yellow 56, turmeric yellow 61, turmeric yellow 65, turmeric yellow 72, turmeric yellow 73, turmeric yellow 76, acid yellow 11 7, turmeric yellow 127, turmeric yellow 158, turmeric yellow 199 etc.
Acid red dye has azogeramine; Xylene Red 6; Xylene Red 7; Xylene Red 9; Azogeramine 4; Azogeramine 7; Acid red 18; Acid red 35; Xylene Red 37; Xylene Red 42; Xylene Red 52; Xylene Red 57; Xylene Red 73; Xylene Red 85; Acid red 87; Acid red 88; Xylene Red 97; Azogeramine 06; Azogeramine 11; Azogeramine 14; Azogeramine 15; Azogeramine 18; Azogeramine 19; Azogeramine 22; Azogeramine 31; Azogeramine 38; Azogeramine 41; Azogeramine 42; Acid red 151; Azogeramine 54 etc.
Acid orange has von Muller's indicator 3, acid orange 7, von Muller's indicator 10, von Muller's indicator 24, von Muller's indicator 33, von Muller's indicator 51, von Muller's indicator 56 etc.
The acid green dyestuff has acid green 1, acid green 3, acid green 9, acid green 16, acid green 20, ACID GREEN 25, acid green 54 etc.
Acid blue dye is like Blue VRS, Acid Blue 7, acid blue 9, Blue VRS 5, acid blue 25, acid blue 27, Acid Blue 40, acid blue 41, acid blue 43, acid blue 45, acid blue 47, acid blue 62, acid blue 80, acid blue 90, acid blue 92, acid blue 93, Acid blue 113, Blue VRS 20, Blue VRS 27, ACID BLUE 129, Blue VRS 38 etc.
Described mordant dyes have media Huang 3, media Huang 5, Metachrome Yellow 0, Metachrome Yellow 2, media Huang 26, media Huang 66, medium red 3, medium red 7, medium red 11, medium red 15, medium red 21, media indigo plant 1, media indigo plant 3, media indigo plant 9, mordant blue 13 etc.
Described reactive dyestuffs have reactive yellow 1, reactive yellow 3, reactive yellow 4, reactive yellow 14, reactive yellow 15, reactive yellow 17, reactive yellow 57, reactive yellow 86, REACTIVE Yellow 145, reactive red 1, reactive red 2, reactive red 3, reactive red 11, reactive red 15, reactive red 23, reactive red 49, reactive red 177, reactive violet 8, reactive blue 4, Reactive Blue 19 100 etc.
Described substantive dyestuff has direct yellow 24, Direct Yellow 26, directly yellow 34, Direct Yellow 44, directly yellow 49, Direct Yellow 50, directly yellow 117, directly yellow 118, directly red 1, directly red 2, directly red 13, directly red 28, directly red 79, directly purple 1, directly purple 12, sun blue 1, sun blue 2, sun blue 6, sun blue 15, sun blue 22, sun blue 80, sun blue 106, sun green 1, sun green 6, sun green 85 etc.
Suitable dyestuff includes but not limited to above-mentioned dyestuff.
The sodium salt of described pigment dyestuff or acid precursor have the sodium salt precursor or the acid precursor of pigment red 4 8:1, Pigment red 52:1, Pigment red 54, Pigment red 55, Pigment red 56, Pigment red 57:1, Pigment red 58:1, Pigment red 64:1, Pigment red 77 etc.
The concrete preparation process of supramolecular structure pigment that polycomponent colour developing negatively charged ion is total to intercalation is following:
A. will contain M
2+, M
3+Nitrate salt or muriate be dissolved in and prepare mixing salt solution, wherein M in the solvent
3+Volumetric molar concentration be 0.025～0.5mol/L, M
2+With M
3+Molar concentration rate be 2～4; Described solvent is the mixture of deionized water or deionized water and polar solvent; M
2+Be divalent-metal ion Mg
2+, Zn
2+, Ni
2+, Ca
2+, Fe
2+Or Cu
2+In any one or two kinds, preferably Mg
2+Or Zn
2+M
3+Be trivalent metal ion Al
3+, Co
3+, Ti
3+, Fe
3+Or Cr
3+In any one or two kinds, preferably Al
3+Described polar solvent is propyl alcohol, terepthaloyl moietie, Ucar 35, butyleneglycol, pentanediol, pinakon, USP Kosher, trihydroxybutane or butantetraol;
B. prepare the alkaline solution that volumetric molar concentration is 0.05～1mol/L, alkaline solution is NaOH, KOH or ammonia soln;
C. be dissolved in after two or more is different colour developing anionic compound mixes and be made into chromophoric solution in the solvent, anionic electric charge molar weight sum and M wherein develop the color
3+Mol ratio is 1.1～1.5, and the molar content of arbitrary colour developing anionic compound in the colour developing anion mixture is 0.02～0.95;
Described solvent is deionized water, polar solvent or the mixture of the two; Concrete selection is looked used colour developing anionic compound and is decided, and described polar solvent is propyl alcohol, terepthaloyl moietie, Ucar 35, butyleneglycol, pentanediol, pinakon, USP Kosher, trihydroxybutane or butantetraol; Described colour developing anionic compound is foregoing compound;
D. three kinds of solution with steps A, B and C configuration mix; Wherein the add-on of alkaline solution should make the pH value of reaction solution be controlled between 4.5～10; 80～200 ℃ with nitrogen protection under stirring reaction 12～48 hours; Filter, wash closely colourless,, obtain the polycomponent colour developing negatively charged ion supramolecular structure pigment of intercalation altogether 90～150 ℃ of dryings 12～24 hours to washing lotion.Wherein three kinds of solution of A, B and C preparation can mix with random order;
Used deionized water all is through taking off CO among steps A, B, C, the D
2The deionized water of handling.
The supramolecular structure pigment that the polycomponent colour developing negatively charged ion that obtains is total to intercalation carries out XRD and FT-IR sign, and the result shows that polycomponent colour developing negatively charged ion has been assembled into stratified material LDHs interlayer.
Advantage of the present invention: the prepared polycomponent colour developing negatively charged ion of the present invention is total to intercalation supramolecular structure pigment color and is different from the anion intercalated supramolecular structure pigment of single colour developing; Its color anionic mol ratio that can develop the color through the difference that modulation inserts hydrotalcite layers is regulated and control, thus the polycomponent colour developing negatively charged ion of preparing a series of different colours intercalation supramolecular structure pigment altogether.Prepared polycomponent colour developing negatively charged ion intercalation supramolecular structure hydrotalcite altogether can be used as the pigment use.The preparation method who is adopted is simple, is convenient to suitability for industrialized production.
Description of drawings:
Fig. 1 is the XRD spectra that the two-pack colour developing negatively charged ion of embodiment 1 preparation is total to intercalation supramolecular structure pigment.
Fig. 2 is the FT-IR spectrogram that the two-pack colour developing negatively charged ion of embodiment 1 preparation is total to intercalation supramolecular structure pigment.
Fig. 3 is the XRD spectra that the two-pack colour developing negatively charged ion of embodiment 2 preparations is total to intercalation supramolecular structure pigment.
Fig. 4 is the FT-IR spectrogram that the two-pack colour developing negatively charged ion of embodiment 2 preparations is total to intercalation supramolecular structure pigment.
Fig. 5 is the XRD spectra that the two-pack colour developing negatively charged ion of embodiment 3 preparations is total to intercalation supramolecular structure pigment.
Fig. 6 is the FT-IR spectrogram that the two-pack colour developing negatively charged ion of embodiment 3 preparations is total to intercalation supramolecular structure pigment.
Embodiment:
Embodiment 1:
Steps A: take by weighing 2.975g (10mmol) Zn (NO
3)
26H
2O, 1.875g (5mmol) Al (NO
3)
39H
2O, be dissolved in 50ml and remove CO
2Deionized water in be made into mixing salt solution.
Step B: take by weighing 1.20g NaOH and be dissolved in 50ml except that CO
2Deionized water in proportionaling alkali-forming solution.
Step C: take by weighing 2.872g (5.225mmol) turmeric yellow 25 and 0.115g (0.275mmol) acid blue 25 and be dissolved in 100ml except that CO
2The middle wiring solution-forming of the mixed solvent formed of deionized water and terepthaloyl moietie (water and terepthaloyl moietie volume ratio are 1: 1, down with).
Step D: the solution of step C preparation is joined in the solution of steps A preparation; Drips of solution with step B preparation under nitrogen protection and stirring is added in the mixing solutions of A and C; Dropwise in 30 minutes, reacted 24 hours down with nitrogen protection at 100 ℃ subsequently, filter, wash closely colourless to washing lotion; At 100 ℃ of dry 24h, obtain a kind of yellow light green supermolecular intercalation structure pigment.XRD and FT-IR analysis revealed turmeric yellow 25 have arrived hydrotalcite layers with the common intercalation of acid blue 25 negatively charged ion.
Embodiment 2:
Steps A: take by weighing 2.975g (10mmol) Zn (NO
3)
26H
2O, 1.875g (5mmol) Al (NO
3)
39H
2O, be dissolved in 50ml and remove CO
2The mixed solvent formed of deionized water and terepthaloyl moietie in be made into mixing solutions.
Step B: take by weighing 1.20g NaOH and be dissolved in 80ml except that CO
2Deionized water in proportionaling alkali-forming solution.
Step C: take by weighing 2.720g (4.95mmol) turmeric yellow 25 and 0.229g (0.55mmol) acid blue 25 and be dissolved in 100ml except that CO
2The mixed solvent formed of deionized water and terepthaloyl moietie in wiring solution-forming.
Step D: the solution of step C preparation is joined in the solution of steps A preparation; Drips of solution with step B preparation under nitrogen protection and stirring is added in the mixing solutions of A and C; Dropwise in 40 minutes, reacted 24 hours down with nitrogen protection at 105 ℃ subsequently, filter, wash closely colourless to washing lotion; At 100 ℃ of dry 24h, obtain a kind of smaragdine(-nus) supermolecular intercalation structure pigment.XRD and FT-IR analysis revealed turmeric yellow 25 have arrived hydrotalcite layers with the common intercalation of acid blue 25 negatively charged ion.
Embodiment 3:
Steps A: take by weighing 2.975g (10mmol) Zn (NO
3)
26H
2O, 1.875g (5mmol) Al (NO
3)
39H
2O, be dissolved in 30ml and remove CO
2Deionized water in be made into mixing salt solution.
Step B: with embodiment 1.
Step C: take by weighing 2.418g (4.4mmol) turmeric yellow 25 and 0.458g (1.1mmol) acid blue 25 and be dissolved in 120ml except that CO
2The mixed solvent formed of deionized water and terepthaloyl moietie in wiring solution-forming.
Step D: the solution of step C preparation is joined in the solution of steps A preparation; Drips of solution with step B preparation under nitrogen protection and stirring is added in the mixing solutions of A and C; Dropwise in 35 minutes, reacted 24 hours down with nitrogen protection at 95 ℃ subsequently, filter, wash closely colourless to washing lotion; At 100 ℃ of dry 24h, obtain a kind of grass green supermolecular intercalation structure pigment.XRD and FT-IR analysis revealed turmeric yellow 25 have arrived hydrotalcite layers with the common intercalation of acid blue 25 negatively charged ion.
Embodiment 4:
Steps A: with embodiment 2.
Step B: take by weighing 1.20g NaOH and be dissolved in 80ml except that CO
2The mixed solvent formed of deionized water and terepthaloyl moietie in proportionaling alkali-forming solution.
Step C: take by weighing 1.209g (2.2mmol) turmeric yellow 25 and 1.374g (3.3mmol) acid blue 25 and be dissolved in 100ml except that CO
2The mixed solvent formed of deionized water and terepthaloyl moietie in wiring solution-forming.
Step D:, behind 90 ℃ of dry 24h, obtain the blue supermolecular intercalation structure pigment of a kind of green glow with embodiment 2.XRD and FT-IR analysis revealed turmeric yellow 25 have arrived hydrotalcite layers with the common intercalation of acid blue 25 negatively charged ion.
Embodiment 5:
Steps A: with embodiment 1.
Step B: with embodiment 1.
Step C: take by weighing 0.7g (1.38mmol) azogeramine and 0.809g (1.38mmol) acid green 20 and be dissolved in 100ml except that CO
2Deionized water in wiring solution-forming.
Step D:, behind 100 ℃ of dry 24h, obtain a kind of yellow supermolecular intercalation structure pigment with embodiment 1.XRD and FT-IR analysis revealed azogeramine and the common intercalation of acid green 20 negatively charged ion have arrived hydrotalcite layers.
Embodiment 6:
Steps A: with embodiment 1.
Step B: with embodiment 1.
Step C: take by weighing 0.624g (1.38mmol) von Muller's indicator 10 and 0.809g (1.38mmol) acid green 20 and be dissolved in 100ml except that CO
2Deionized water in wiring solution-forming.
Step D: the solution with steps A and B preparation under nitrogen protection and stirring is added drop-wise in the solution of step C configuration simultaneously; Dropwise in the 30min; Reacted 24 hours down with nitrogen protection at 100 ℃ subsequently; Filter, wash closely colourless, behind 100 ℃ of dry 24h, obtain a kind of yellow supermolecular intercalation structure pigment to washing lotion.XRD and FT-IR analysis revealed von Muller's indicator 10 have arrived hydrotalcite layers with the common intercalation of acid green 20 negatively charged ion.
Embodiment 7:
Steps A: with embodiment 1.
Step B: with embodiment 1.
Step C: take by weighing 0.575g (1.38mmol) acidic intermedium yellow 3 and 0.694g (1.38mmol) MORDANT BLUE 9 and be dissolved in 100ml except that CO
2Deionized water in wiring solution-forming.
Step D:, behind 100 ℃ of dry 24h, obtain a kind of green supermolecular intercalation structure pigment with embodiment 6.XRD and FT-IR analysis revealed acidic intermedium yellow 3 and the common intercalation of MORDANT BLUE 9 negatively charged ion have arrived hydrotalcite layers.
Embodiment 8:
Steps A: with embodiment 1.
Step B: with embodiment 1.
Step C: take by weighing 0.921g (1.38mmol) reactive yellow 86 and 0.849g (1.38mmol) reactive red 2 and be dissolved in 100ml except that CO
2The mixed solvent formed of deionized water and terepthaloyl moietie in wiring solution-forming.
Step D:, behind 100 ℃ of dry 24h, obtain a kind of orange supermolecular intercalation structure pigment with embodiment 1.XRD and FT-IR analysis revealed reactive yellow 86 have arrived hydrotalcite layers with the common intercalation of reactive red 2 negatively charged ion.
Embodiment 9:
Steps A: with embodiment 1.
Step B: with embodiment 1.
Step C: take by weighing 0.849g (1.38mmol) reactive red 2 and 0.94g (1.38mmol) reactive blue 4 and be dissolved in 100ml except that CO
2The mixed solvent formed of deionized water and terepthaloyl moietie in wiring solution-forming.
Step D:, behind 100 ℃ of dry 24h, obtain a kind of yellow supermolecular intercalation structure pigment with embodiment 6.XRD and FT-IR analysis revealed reactive red 2 have arrived hydrotalcite layers with the common intercalation of reactive blue 4 negatively charged ion.
Embodiment 10:
Steps A: with embodiment 1.
Step B: with embodiment 1.
Step C: take by weighing 0.775g (1.38mmol) direct yellow 24 and 1.023g (1.38mmol) sun blue 106 and be dissolved in 100ml except that CO
2The mixed solvent formed of deionized water and terepthaloyl moietie in wiring solution-forming.
Step D:, behind 100 ℃ of dry 24h, obtain a kind of green supermolecular intercalation structure pigment with embodiment 1.XRD and FT-IR analysis revealed directly Huang 24 have arrived hydrotalcite layers with the common intercalation of sun blue 106 negatively charged ion.
Embodiment 11:
Steps A: with embodiment 1.
Step B: with embodiment 1.
Step C: take by weighing 0.849g (1.38mmol) direct red 2 and 1.059g (1.38mmol) sun green 1 and be dissolved in 100ml except that CO
2The mixed solvent formed of deionized water and terepthaloyl moietie in wiring solution-forming.
Step D:, behind 100 ℃ of dry 24h, obtain a kind of yellow supermolecular intercalation structure pigment with embodiment 6.XRD and FT-IR analysis revealed direct red 2 and the common intercalation of sun green 1 negatively charged ion have arrived hydrotalcite layers.
Embodiment 12:
Steps A: with embodiment 1.
Step B: with embodiment 1.
Step C: take by weighing 1.006g (1.38mmol) direct purple 1 and 1.116g (1.38mmol) acid green 54 and be dissolved in 100ml except that CO
2Deionized water in wiring solution-forming.
Step D:, behind 100 ℃ of dry 24h, obtain a kind of blue supermolecular intercalation structure pigment with embodiment 6.XRD and FT-IR analysis revealed directly purple 1 have arrived hydrotalcite layers with the common intercalation of acid green 54 negatively charged ion.
Embodiment 13:
Steps A: with embodiment 1.
Step B: with embodiment 1.
Step C: the sodium salt that takes by weighing 0.505g (1.38mmol) acidic intermedium yellow 10 and 0.641g (1.38mmol) pigment red 4 8:1 is dissolved in 100ml and removes CO
2The mixed solvent of deionized water and terepthaloyl moietie in wiring solution-forming.
Step D:, behind 100 ℃ of dry 24h, obtain a kind of orange supermolecular intercalation structure pigment with embodiment 6.The common intercalation of negatively charged ion of XRD and FT-IR analysis revealed acidic intermedium yellow 10 and pigment red 4 8:1 has arrived hydrotalcite layers.
Claims (4)
1. a polycomponent colour developing negatively charged ion is total to intercalation supramolecular structure pigment, and its chemical general formula is:
M
2+ 1-xM
3+ x(OH)
2(A
n-)
x/n·mH
2O
0.1≤x≤0.5 wherein, m is an interlayer crystal water molecule number; M
2+Be divalent-metal ion Mg
2+, Zn
2+, Ni
2+, Ca
2+, Fe
2+Or Cu
2+In any one or two kinds; M
3+Be trivalent metal ion Al
3+, Co
3+, Ti
3+, Fe
3+Or Cr
3+In any one or two kinds; A
N-Be two or more colour developing negatively charged ion;
Said colour developing anionic compound be the branch dyestuff or with the pigment dyestuff precursor, wherein dyestuff has matching stain, mordant dyes, reactive dyestuffs, substantive dyestuff; The pigment dyestuff precursor is the sodium salt or the acid precursor of pigment dyestuff.
2. polycomponent colour developing negatively charged ion according to claim 1 is intercalation supramolecular structure pigment altogether, it is characterized in that M
2+Be Mg
2+Or Zn
2+, M
3+Be Al
3+
Described matching stain has turmeric yellow, Xylene Red, von Muller's indicator, acid green, acid blue; Wherein acid yellow dye has quinoline yellow, acid yellow 11, turmeric yellow 13, turmeric yellow 14, turmeric yellow 17, turmeric yellow 19, turmeric yellow 25, quinoline yellow 6, quinoline yellow 8, turmeric yellow 40, turmeric yellow 42, turmeric yellow 44, turmeric yellow 49, turmeric yellow 56, turmeric yellow 61, turmeric yellow 65, turmeric yellow 72, turmeric yellow 73, turmeric yellow 76, acid yellow 11 7, turmeric yellow 127, turmeric yellow 158 or turmeric yellow 199;
Acid red dye has azogeramine; Xylene Red 6; Xylene Red 7; Xylene Red 9; Azogeramine 4; Azogeramine 7; Acid red 18; Acid red 35; Xylene Red 37; Xylene Red 42; Xylene Red 52; Xylene Red 57; Xylene Red 73; Xylene Red 85; Acid red 87; Acid red 88; Xylene Red 97; Azogeramine 06; Azogeramine 11; Azogeramine 14; Azogeramine 15; Azogeramine 18; Azogeramine 19; Azogeramine 22; Azogeramine 31; Azogeramine 38; Azogeramine 41; Azogeramine 42; Acid red 151 or azogeramine 54;
Acid orange has von Muller's indicator 3, acid orange 7, von Muller's indicator 10, von Muller's indicator 24, von Muller's indicator 33, von Muller's indicator 51 or von Muller's indicator 56;
The acid green dyestuff has acid green 1, acid green 3, acid green 9, acid green 16, acid green 20, ACID GREEN 25 or acid green 54 etc.;
Acid blue dye is like Blue VRS, Acid Blue 7, acid blue 9, Blue VRS 5, acid blue 25, acid blue 27, Acid Blue 40, acid blue 41, acid blue 43, acid blue 45, acid blue 47, acid blue 62, acid blue 80, acid blue 90, acid blue 92, acid blue 93, Acid blue 113, Blue VRS 20, Blue VRS 27, ACID BLUE 129 or Blue VRS 38;
Described mordant dyes have media Huang 3, media Huang 5, Metachrome Yellow 0, Metachrome Yellow 2, media Huang 26, media Huang 66, medium red 3, medium red 7, medium red 11, medium red 15, medium red 21, media indigo plant 1, media indigo plant 3, media indigo plant 9, mordant blue 13 etc.;
Described reactive dyestuffs have reactive yellow 1, reactive yellow 3, reactive yellow 4, reactive yellow 14, reactive yellow 15, reactive yellow 17, reactive yellow 57, reactive yellow 86, REACTIVE Yellow 145, reactive red 1, reactive red 2, reactive red 3, reactive red 11, reactive red 15, reactive red 23, reactive red 49, reactive red 177, reactive violet 8, reactive blue 4 or Reactive Blue 19 100;
Described substantive dyestuff has direct yellow 24, Direct Yellow 26, directly yellow 34, Direct Yellow 44, directly yellow 49, Direct Yellow 50, directly yellow 117, directly yellow 118, directly red 1, directly red 2, directly red 13, directly red 28, directly red 79, directly purple 1, directly purple 12, sun blue 1, sun blue 2, sun blue 6, sun blue 15, sun blue 22, sun blue 80, sun blue 106, sun green 1, sun green 6 or sun green 85;
The sodium salt of described pigment dyestuff or acid precursor have the sodium salt precursor or the acid precursor of pigment red 4 8:1, Pigment red 52:1, Pigment red 54, Pigment red 55, Pigment red 56, Pigment red 57:1, Pigment red 58:1, Pigment red 64:1, Pigment red 77.
3. one kind prepares the described polycomponent colour developing of the claim 1 negatively charged ion method of intercalation supramolecular structure pigment altogether, and concrete steps are following:
A. will contain M
2+, M
3+Nitrate salt or muriate be dissolved in and prepare mixing salt solution, wherein M in the solvent
3+Volumetric molar concentration be 0.025～0.5mol/L, M
2+With M
3+Molar concentration rate be 2～4; Described solvent is the mixture of deionized water or deionized water and polar solvent; M
2+Be divalent-metal ion Mg
2+, Zn
2+, Ni
2+, Ca
2+, Fe
2+Or Cu
2+In any one or two kinds; M
3+Be trivalent metal ion Al
3+, Co
3+, Ti
3+, Fe
3+Or Cr
3+In any one or two kinds; Described polar solvent is propyl alcohol, terepthaloyl moietie, Ucar 35, butyleneglycol, pentanediol, pinakon, USP Kosher, trihydroxybutane or butantetraol;
B. prepare the alkaline solution that volumetric molar concentration is 0.05～1mol/L, alkaline solution is NaOH, KOH or ammonia soln;
C. be dissolved in after two or more is different colour developing anionic compound mixes and be made into chromophoric solution in the solvent, anionic electric charge molar weight sum and M wherein develop the color
3+Mol ratio is 1.1～1.5, and the molar content of arbitrary colour developing anionic compound in the colour developing anion mixture is 0.02～0.95;
Described solvent is deionized water, polar solvent or the mixture of the two; Concrete selection is looked used colour developing anionic compound and is decided, and described polar solvent is propyl alcohol, terepthaloyl moietie, Ucar 35, butyleneglycol, pentanediol, pinakon, USP Kosher, trihydroxybutane or butantetraol; Described colour developing anionic compound is the compound described in the claim 2 and 2;
D. three kinds of solution with steps A, B and C configuration mix; Wherein the add-on of alkaline solution should make the pH value of reaction solution be controlled between 4.5～10; 80～200 ℃ with nitrogen protection under stirring reaction 12～48 hours; Filter, wash closely colourless,, obtain the polycomponent colour developing negatively charged ion supramolecular structure pigment of intercalation altogether 90～150 ℃ of dryings 12～24 hours to washing lotion.Wherein three kinds of solution of A, B and C preparation can mix with random order;
Used deionized water all is through taking off CO among steps A, B, C, the D
2The deionized water of handling.
4. the polycomponent colour developing negatively charged ion method of intercalation supramolecular structure pigment altogether for preparing according to claim 3 is characterized in that the described M of steps A
2+Be Mg
2+Or Zn
2+, M
3+Be Al
3+
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| CN103319913A (en) * | 2013-06-18 | 2013-09-25 | 安科智慧城市技术（中国）有限公司 | Preparation method of dye intercalation hydrotalcite-like nanometer composite material |
| CN103965654A (en) * | 2014-04-30 | 2014-08-06 | 北京化工大学 | Light-fastness pigment with super-molecular intercalated structure and preparation method thereof |
| CN104049051A (en) * | 2014-06-18 | 2014-09-17 | 南京麦思德餐饮管理有限公司 | Pretreatment method for detecting rose pink R in candies |
| CN105176134A (en) * | 2015-09-25 | 2015-12-23 | 恒升化工有限公司 | High-dissolvability acid yellow dye and preparation method thereof |
| CN105504876A (en) * | 2015-11-27 | 2016-04-20 | 天津德凯化工股份有限公司 | Red liquid dye composition and preparation method thereof |
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| CN103319913A (en) * | 2013-06-18 | 2013-09-25 | 安科智慧城市技术（中国）有限公司 | Preparation method of dye intercalation hydrotalcite-like nanometer composite material |
| CN103965654A (en) * | 2014-04-30 | 2014-08-06 | 北京化工大学 | Light-fastness pigment with super-molecular intercalated structure and preparation method thereof |
| CN103965654B (en) * | 2014-04-30 | 2016-08-17 | 北京化工大学 | A kind of supermolecular intercalation structure of resistance to light type pigment and preparation method thereof |
| CN104049051A (en) * | 2014-06-18 | 2014-09-17 | 南京麦思德餐饮管理有限公司 | Pretreatment method for detecting rose pink R in candies |
| CN105176134A (en) * | 2015-09-25 | 2015-12-23 | 恒升化工有限公司 | High-dissolvability acid yellow dye and preparation method thereof |
| CN105504876A (en) * | 2015-11-27 | 2016-04-20 | 天津德凯化工股份有限公司 | Red liquid dye composition and preparation method thereof |
| CN105504876B (en) * | 2015-11-27 | 2020-05-01 | 天津德凯化工股份有限公司 | Red liquid dye composition and preparation method thereof |
| CN110408314A (en) * | 2019-08-05 | 2019-11-05 | 宜兴汉光高新石化有限公司 | A kind of interior preparation method with solvent-free static electricity conductive anticorrosive paint of oil storage tank |
| CN110408314B (en) * | 2019-08-05 | 2021-06-25 | 宜兴汉光高新石化有限公司 | Preparation method of solvent-free static conductive anticorrosive paint for oil storage tank |
| CN110982299A (en) * | 2019-12-11 | 2020-04-10 | 西华大学 | Pigment system imitating spectral characteristics of natural vegetation and preparation method |
| CN110982299B (en) * | 2019-12-11 | 2021-06-18 | 西华大学 | Pigment system imitating spectral characteristics of natural vegetation and preparation method |
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