CN109370249A - A kind of preparation method of Lithol Red - Google Patents
A kind of preparation method of Lithol Red Download PDFInfo
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- CN109370249A CN109370249A CN201811382489.8A CN201811382489A CN109370249A CN 109370249 A CN109370249 A CN 109370249A CN 201811382489 A CN201811382489 A CN 201811382489A CN 109370249 A CN109370249 A CN 109370249A
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- VVNRQZDDMYBBJY-UHFFFAOYSA-M sodium 1-[(1-sulfonaphthalen-2-yl)diazenyl]naphthalen-2-olate Chemical compound [Na+].C1=CC=CC2=C(S([O-])(=O)=O)C(N=NC3=C4C=CC=CC4=CC=C3O)=CC=C21 VVNRQZDDMYBBJY-UHFFFAOYSA-M 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 66
- 239000000243 solution Substances 0.000 claims abstract description 42
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims abstract description 33
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims abstract description 33
- 238000005859 coupling reaction Methods 0.000 claims abstract description 33
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims abstract description 33
- 230000008878 coupling Effects 0.000 claims abstract description 26
- 238000010168 coupling process Methods 0.000 claims abstract description 26
- 125000000664 diazo group Chemical group [N-]=[N+]=[*] 0.000 claims abstract description 26
- 239000002253 acid Substances 0.000 claims abstract description 19
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical class [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims abstract description 15
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 claims abstract description 12
- 229910001626 barium chloride Inorganic materials 0.000 claims abstract description 12
- 235000010288 sodium nitrite Nutrition 0.000 claims abstract description 10
- 238000004090 dissolution Methods 0.000 claims abstract description 8
- 239000004744 fabric Substances 0.000 claims abstract description 8
- KSTGSVANFMJGGB-UHFFFAOYSA-N 2-ethylnaphthalen-1-ol Chemical class C1=CC=CC2=C(O)C(CC)=CC=C21 KSTGSVANFMJGGB-UHFFFAOYSA-N 0.000 claims abstract description 7
- 206010067171 Regurgitation Diseases 0.000 claims abstract description 7
- 239000012047 saturated solution Substances 0.000 claims abstract description 7
- 238000006277 sulfonation reaction Methods 0.000 claims abstract description 7
- 150000007513 acids Chemical class 0.000 claims abstract 2
- 238000003756 stirring Methods 0.000 claims description 21
- RGCKGOZRHPZPFP-UHFFFAOYSA-N alizarin Chemical compound C1=CC=C2C(=O)C3=C(O)C(O)=CC=C3C(=O)C2=C1 RGCKGOZRHPZPFP-UHFFFAOYSA-N 0.000 claims description 7
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- -1 sodium alkyl benzene Chemical class 0.000 claims description 4
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 3
- 239000008117 stearic acid Substances 0.000 claims description 3
- 229940077388 benzenesulfonate Drugs 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000004094 surface-active agent Substances 0.000 claims description 2
- 125000000129 anionic group Chemical group 0.000 claims 2
- 235000008331 Pinus X rigitaeda Nutrition 0.000 claims 1
- 235000011613 Pinus brutia Nutrition 0.000 claims 1
- 241000018646 Pinus brutia Species 0.000 claims 1
- 239000002304 perfume Substances 0.000 claims 1
- 239000000049 pigment Substances 0.000 abstract description 36
- 238000000034 method Methods 0.000 abstract description 10
- 239000002245 particle Substances 0.000 abstract description 9
- 230000008569 process Effects 0.000 abstract description 9
- 239000003973 paint Substances 0.000 abstract description 6
- 239000003945 anionic surfactant Substances 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 15
- 239000012954 diazonium Substances 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-O diazynium Chemical compound [NH+]#N IJGRMHOSHXDMSA-UHFFFAOYSA-O 0.000 description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 9
- 238000010792 warming Methods 0.000 description 7
- 239000003921 oil Substances 0.000 description 6
- 229960000583 acetic acid Drugs 0.000 description 5
- 239000011435 rock Substances 0.000 description 5
- 238000004040 coloring Methods 0.000 description 4
- 239000000975 dye Substances 0.000 description 4
- 239000012362 glacial acetic acid Substances 0.000 description 4
- GWIAAIUASRVOIA-UHFFFAOYSA-N 2-aminonaphthalene-1-sulfonic acid Chemical compound C1=CC=CC2=C(S(O)(=O)=O)C(N)=CC=C21 GWIAAIUASRVOIA-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- IOVCWXUNBOPUCH-UHFFFAOYSA-N Nitrous acid Chemical compound ON=O IOVCWXUNBOPUCH-UHFFFAOYSA-N 0.000 description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000002552 dosage form Substances 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 230000003311 flocculating effect Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 159000000009 barium salts Chemical group 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000012860 organic pigment Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000001054 red pigment Substances 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B29/00—Monoazo dyes prepared by diazotising and coupling
- C09B29/10—Monoazo dyes prepared by diazotising and coupling from coupling components containing hydroxy as the only directing group
- C09B29/103—Monoazo dyes prepared by diazotising and coupling from coupling components containing hydroxy as the only directing group of the naphthalene series
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B29/00—Monoazo dyes prepared by diazotising and coupling
- C09B29/0014—Monoazo dyes prepared by diazotising and coupling from diazotized aminonaphthalene
-
- 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
-
- 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
- C09D7/41—Organic pigments; Organic dyes
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The present invention provides a kind of preparation method of Lithol Red, it is related to pigment technology field, the following steps are included: (1), which configures coupling solution, obtains coupling solution by weight by 3-5.6 parts of liquid alkaline, 3-5 parts of ethyl naphthols, 0.6-1.5 parts of anionic surfactant mixed dissolutions；(2) diazo liquid is prepared, 3-4.5 parts of liquid alkaline, 3-4 parts of tobias acids, 3-4 parts of sulfonation acid regurgitations, the cold acid of 2-4 parts of cloth are uniformly mixed by weight, 0.6-3 parts of hydrochloric acid, 1.5 ~ 2.8 parts of sodium nitrites are added, carries out diazo reaction, obtains diazo liquid；(3) by weight, 2-4 parts of liquid alkaline, 2-3 parts of rosin are mixed, obtains rosin liquid；(4) coupling solution, diazo liquid are mixed, carries out coupling reaction, add rosin liquid, barium chloride saturated solution, alchlor is added when adjusting pH value=7.5-8.0, obtains Lithol Red.The pigment that the present invention prepares ink, paint use process in system will not flocculate, pigment will not separate, and the depth of color is uniform, and pigment particles refinement, partial size is small.
Description
Technical field
The present invention relates to pigment technology fields, and in particular to a kind of preparation method of Lithol Red.
Background technique
Pigment used in ink is the raw material for instigating ink colour generation, have it is not soluble in water, with excellent alcohol resistance
Feature.Pigment is the organic or inorganic colored compound of coloured not soluble in water and common organic solvents, but and not all
Colored substance all can be used as organic pigment use, and coloring matter will become pigment, they must have performance:
1) bright in luster, it can assign by coloring object (or substrate) firm color；
2) not soluble in water, organic solvent or applicating medium；
3) it is easy to evenly dispersed in the application, and not by the physics of applicating medium and chemical affect in entire dispersion process,
Retain their itself intrinsic crystal structure；
4) sun-resistant, weatherability, heat-resisting, acid and alkali-resistance and organic solvent-resistant.
Lithol Red is also known as 2- (2- hydroxyl -1- naphthylazo) -1-naphthalene sulfonic aicd barium, it is a kind of dyestuff and pigment, slightly soluble
In ethyl alcohol, acetone and hot water；It is in concentrated sulfuric acid feux rouges purple, is changed into feux rouges brown precipitate after dilution；Meeting concentrated nitric acid is
Brown-red solution；It is slightly soluble in sodium hydrate aqueous solution, in alcoholic solution plus hydrochloric acid becomes brown purple.The pigment variety is barium salt color
It forms sediment, provides neutral feux rouges, since heat-resistant stability is undesirable, limit application in the plastic；It is mainly used in printing ink coloring,
In particular for publication gravure ink, the dosage form of resinification processing can reduce its bronzing phenomenon；Dedicated dosage form is suitable for aqueous printing ink；
The trade names of launch are up to as many as 54 kinds.More economical type pigment variety.It is mainly used for watercolor, the oil of ink and school supply and stationery
The coloring pigment of coloured silk etc., it can also be used to coating.
The Lithol Red pigment produced in the prior art forms biggish pigment aggregation block easily there is a phenomenon where flocculating,
Speed slows down in eddy motion, will cause pigment separation, shoals sometimes, form piebald sometimes, the meeting in normal use
There is uneven color, the phenomenon of pigment thickness unevenness.
Summary of the invention
In view of this, the present invention provides a kind of preparation method of Lithol Red, the pigment prepared is in ink, paint
System will not flocculate in use process, and pigment will not separate, and the depth of color is uniform.
The present invention is a kind of preparation method of Lithol Red, comprising the following steps:
(1) configure coupling solution, at 15-20 DEG C stir in the case where by weight by 3-5.6 part mass fractions be 25-28%
Liquid alkaline, 3-5 parts of ethyl naphthols, 0.6-1.5 parts of anionic surfactant mixed dissolutions, be completely dissolved, when solution is transparent, will
The temperature of solution is reduced to 15-20 DEG C, can reduce temperature by mode on the rocks, obtain coupling solution, anionic surfactant
For one of turkey red oil, sodium alkyl benzene sulfonate, stearic acid or a variety of；
(2) diazo liquid is prepared, in 25-30 DEG C of bottom water, it is 25-28%'s that 1.5-2.5 by weight parts of mass fraction, which is added,
Liquid alkaline, 3-4 part tobias acid, 3-4 parts of sulfonation acid regurgitations, the 2-4 parts of cold acid of cloth are opened stirring adjustment electric machine frequency 25Hz, are uniformly mixed, will
The temperature of mixed liquor is adjusted to -1 ~ 0 DEG C, and it is 24-26% that 3-5 parts of mass fractions, which are added, in the case where being 50Hz or so in electric machine frequency
Hydrochloric acid, 2.4 ~ 3.8 parts of sodium nitrites, carry out diazo reaction, obtain diazo liquid, the addition of sodium nitrite will be used as far as possible rapidly
PH test paper and KI test paper check diazonium terminal, and KI test paper is more blue, and pH test paper is redder, indicate that reaction terminates, adjustment temperature is -1~
0 DEG C, it is stand-by to continue stirring；
(3) by weight, 2-4 parts of liquid alkaline, 2-3 parts of rosin are mixed, obtains rosin liquid, first liquid alkaline is added to the water, so
After be warming up to 85-90 DEG C, rosin is added, continues to be warming up to 90-95 DEG C, stirring to rosin is completely dissolved；
(4) it is quickly mixed with diazo liquid after coupling solution being sieved, diazonium is not excessive, carries out coupling reaction, reaction temperature 5-8
DEG C, coupling finishes pH=12.4-12.6 or so, adds the rosin liquid, barium chloride saturated solution, and barium chloride should first add water
It is then added in solution system after dissolution, alchlor is added when adjusting pH value=7.5-8.0, adjusting pH value can be used ice vinegar
Acid obtains Lithol Red.
The various functions of surfactant are mainly manifested in the property on the surface, liquid-liquid interface and liquid-solid interface that change liquid
Matter, wherein table (boundary) face property of liquid is most important.Change the specific surface of system intermediate ion using anionic surfactant
Can, it can be mutually exclusive between particle, it can be effectively prevent the aggregation of particle in system, pigment can guaranteed in the process used
The stability of middle guarantee system, does not flocculate.There is diffusion, wetting action using turkey red oil, can be improved dyestuff to fabric
Permeability and dyefastness, it is also possible to make the defoaming agent of dyestuff, pigment and dyestuff intermediate, turkey red oil is optimal in the present invention
Activating agent, can defoam, while improving the fastness of the color of pigment.
Rosin belongs to pigment derivative, and the significant change of color will not be generated after being added in pigment, while can rely on again
Van der Waals force is more securely adsorbed on processed granules of pigments.Rosin, which is added, to be adsorbed in surface of pigments with anchorage, together
When in conjunction with the pigment carrier in system, play three-dimensional inhibition, hinder close to each other between pigment particles, reduce particle
Aggtegation, improvement reach good mobility, the good mobility of system, conducive to pigment is being prepared during the grinding process
When, be conducive to refine particle during grinding refinement.It is also possible to prevent the crystallization of the pigment in heat drying process simultaneously,
It can guarantee the fastness of pigment stability in use and paint color.The molecular weight for increasing pigment, is added simultaneously
Dispersion effect in dispersing agent enhancing system, prevents particle from re-uniting.
The pigment that the present invention prepares ink, paint use process in system will not flocculate, pigment will not divide
From the depth of color is uniform, pigment particles refinement, and partial size is small.
Specific embodiment
The present invention will be described in detail With reference to embodiment.
Embodiment one
A kind of preparation method of Lithol Red, comprising the following steps:
(1) configure coupling solution, at 15 DEG C stir in the case where by weight by 3 parts of mass fractions be 25-28% liquid alkaline, 3
Part ethyl naphthol, 0.6 part of turkey red oil, mixed dissolution is completely dissolved, and when solution is transparent, the temperature of solution is reduced to 15-20 DEG C,
Temperature can be reduced by mode on the rocks, obtain coupling solution；
(2) diazo liquid is prepared, in 25 DEG C of bottom water, liquid alkaline, 3 parts that 1.5 parts of mass fractions by weight are 25% is added and spits
Family name's acid, 3 parts of sulfonation acid regurgitations, 2 parts of cold acid of cloth open stirring adjustment electric machine frequency 25Hz, are uniformly mixed, the temperature of mixed liquor is adjusted
It is -1 DEG C, the hydrochloric acid, 2.4 parts of sodium nitrites that 3 parts of mass fractions are 24% is added in electric machine frequency in the case where being 50Hz or so, into
Row diazo reaction obtains diazo liquid, and the addition of sodium nitrite will check diazonium terminal with pH test paper and KI test paper as far as possible rapidly,
KI test paper is more blue, and pH test paper is redder, indicates that reaction terminates, and adjustment temperature is -1 DEG C, and it is stand-by to continue stirring；
(3) by weight, 2 parts of liquid alkaline, 2 parts of rosin are mixed, obtains rosin liquid, first liquid alkaline is added to the water, then rises
Rosin is added to 85 DEG C in temperature, continues to be warming up to 90 DEG C, stirring to rosin is completely dissolved；
(4) it quickly being mixed with diazo liquid after coupling solution being sieved, diazonium is not excessive, carries out coupling reaction, and reaction temperature is 5 DEG C,
Coupling finishes pH=12.4-12.6 or so, adds the rosin liquid, barium chloride saturated solution, and barium chloride should be first plus water-soluble
It is then added in solution system after solution, alchlor is added when adjusting pH value=7.5, adjusting pH value can be used glacial acetic acid, obtain
Lithol Red.
Embodiment two
A kind of preparation method of Lithol Red, comprising the following steps:
(1) configure coupling solution, at 20 DEG C stir in the case where by weight by 5.6 parts of mass fractions be 28% liquid alkaline, 5
Part ethyl naphthol, 1.5 parts of sodium alkyl benzene sulfonates, mixed dissolution is completely dissolved, and when solution is transparent, the temperature of solution is reduced to 20
DEG C, temperature can be reduced by mode on the rocks, obtain coupling solution；
(2) diazo liquid is prepared, in 30 DEG C of bottom water, the liquid alkaline, 4 parts of Tu Shi that 2 parts of mass fractions by weight are 28% is added
Acid, 4 parts of sulfonation acid regurgitations, 4 parts of cold acid of cloth open stirring adjustment electric machine frequency 25Hz, are uniformly mixed, the temperature of mixed liquor is adjusted to
0 DEG C, the hydrochloric acid, 2.8 parts of sodium nitrites that 4 parts of mass fractions are 26% is added in electric machine frequency in the case where being 50Hz or so, carries out weight
Nitrogen reaction, obtains diazo liquid, and the addition of sodium nitrite will check diazonium terminal, KI examination with pH test paper and KI test paper as far as possible rapidly
Paper is more blue, and pH test paper is redder, indicates that reaction terminates, and adjustment temperature is 0 DEG C, and it is stand-by to continue stirring；
(3) by weight, 4 parts of liquid alkaline, 3 parts of rosin are mixed, obtains rosin liquid, first liquid alkaline is added to the water, then rises
Rosin is added to 90 DEG C in temperature, continues to be warming up to 95 DEG C, stirring to rosin is completely dissolved；
(4) it quickly being mixed with diazo liquid after coupling solution being sieved, diazonium is not excessive, carries out coupling reaction, and reaction temperature is 8 DEG C,
Coupling finishes pH=12.4-12.6 or so, adds the rosin liquid, barium chloride saturated solution, and barium chloride should be first plus water-soluble
It is then added in solution system after solution, alchlor is added when adjusting pH value=8.0, adjusting pH value can be used glacial acetic acid, obtain
Lithol Red.
Embodiment three
A kind of preparation method of Lithol Red, comprising the following steps:
(1) configure coupling solution, at 18 DEG C stir in the case where by weight by 5 parts of mass fractions be 26% liquid alkaline, 4 parts
Ethyl naphthol, 1 part of stearic acid, mixed dissolution is completely dissolved, and when solution is transparent, the temperature of solution is reduced to 18 DEG C, can be passed through
Mode on the rocks reduces temperature, obtains coupling solution；
(2) diazo liquid is prepared, in 26 DEG C of bottom water, the liquid alkaline, 3.5 parts that 2.5 parts of mass fractions by weight are 26% is added
Tobias acid, 3.5 parts of sulfonation acid regurgitations, 3 parts of cold acid of cloth are opened stirring adjustment electric machine frequency 25Hz, are uniformly mixed, by the temperature of mixed liquor
It is adjusted to -0.5 DEG C, the hydrochloric acid, 3.8 parts of nitrous acid that 5 parts of mass fractions are 25% is added in electric machine frequency in the case where being 50Hz or so
Sodium carries out diazo reaction, obtains diazo liquid, and the addition of sodium nitrite will check diazonium with pH test paper and KI test paper as far as possible rapidly
Terminal, KI test paper is more blue, and pH test paper is redder, indicates that reaction terminates, and adjustment temperature is -0.5 DEG C, and it is stand-by to continue stirring；
(3) by weight, 3 parts of liquid alkaline, 2.5 parts of rosin are mixed, obtains rosin liquid, first liquid alkaline is added to the water, then
86 DEG C are warming up to, rosin is added, continues to be warming up to 92 DEG C, stirring to rosin is completely dissolved；
(4) it quickly being mixed with diazo liquid after coupling solution being sieved, diazonium is not excessive, carries out coupling reaction, and reaction temperature is 7 DEG C,
Coupling finishes pH=12.4-12.6 or so, adds the rosin liquid, barium chloride saturated solution, and barium chloride should be first plus water-soluble
It is then added in solution system after solution, alchlor is added when adjusting pH value=7.8, adjusting pH value can be used glacial acetic acid, obtain
Lithol Red.
Example IV
A kind of preparation method of Lithol Red, comprising the following steps:
(1) configure coupling solution, at 20 DEG C stir in the case where by weight by 4 parts of mass fractions be 25% liquid alkaline, 4.5
Part ethyl naphthol, 1.5 parts of turkey red oils, mixing are completely dissolved, when solution is transparent, the temperature of solution are reduced to 20 DEG C, can be passed through
Mode on the rocks reduces temperature, obtains coupling solution；
(2) diazo liquid is prepared, in 25 DEG C of bottom water, the liquid alkaline, 3.3 parts that 1.8 parts of mass fractions by weight are 25% is added
Tobias acid, 3 parts of sulfonation acid regurgitations, 4 parts of cold acid of cloth are opened stirring adjustment electric machine frequency 25Hz, are uniformly mixed, by the temperature tune of mixed liquor
Whole is -1 DEG C, and the hydrochloric acid, 3.2 parts of nitrous acid that 4.2 parts of mass fractions are 24% is added in electric machine frequency in the case where being 50Hz or so
Sodium carries out diazo reaction, obtains diazo liquid, and the addition of sodium nitrite will check diazonium with pH test paper and KI test paper as far as possible rapidly
Terminal, KI test paper is more blue, and pH test paper is redder, indicates that reaction terminates, and adjustment temperature is -1 DEG C, and it is stand-by to continue stirring；
(3) by weight, 3 parts of liquid alkaline, 3 parts of rosin are mixed, obtains rosin liquid, first liquid alkaline is added to the water, then rises
Rosin is added to 85 DEG C in temperature, continues to be warming up to 93 DEG C, stirring to rosin is completely dissolved；
(4) it quickly being mixed with diazo liquid after coupling solution being sieved, diazonium is not excessive, carries out coupling reaction, and reaction temperature is 6 DEG C,
Coupling finishes pH=12.4-12.6 or so, adds the rosin liquid, barium chloride saturated solution, and barium chloride should be first plus water-soluble
It is then added in solution system after solution, alchlor is added when adjusting pH value=8.0, adjusting pH value can be used glacial acetic acid, obtain
Lithol Red.
The Lithol Red that embodiment one to example IV is prepared is having preferable dispersibility, does not go out in use process
The phenomenon that now flocculating.
The pigment that the present invention prepares ink, paint use process in system will not flocculate, pigment will not divide
From the depth of color is uniform in use process, and pigment particles refinement, partial size is small, and the fastness of paint color is strong, is used for a long time
It is not in fade.And production cost is low, it is environmentally friendly.
The present invention is not limited to above-mentioned specific embodiment, and the invention may be variously modified and varied.All foundations
Technical spirit of the invention should be included in the present invention to embodiment of above any modification, equivalent replacement, improvement and so on
Protection scope.
Claims (7)
1. a kind of preparation method of Lithol Red, which comprises the following steps:
Coupling solution is configured, in the case of stirring by weight by 3-5.6 parts of liquid alkaline, 3-5 parts of ethyl naphthols, 0.6-1.5 parts of yin
Ionic surface active agent mixed dissolution, obtains coupling solution；
Diazo liquid is prepared, it is by weight that 1.5-2.5 parts of liquid alkaline, 3-4 parts of tobias acids, 3-4 parts of sulfonation acid regurgitations, 2-4 parts of cloth are cold
Acid is uniformly mixed, and the temperature of mixed liquor is adjusted to -1 ~ 0 DEG C, 3-5 parts of hydrochloric acid, 2.4 ~ 3.8 parts of sodium nitrites are added, carries out weight
Nitrogen reaction, obtains diazo liquid；
By weight, 1-1.5 parts of liquid alkaline, 2-3 parts of rosin are mixed, obtains rosin liquid；
Coupling solution, diazo liquid are mixed, coupling reaction is carried out, reaction temperature is 5-8 DEG C, adds the rosin liquid, barium chloride
Saturated solution is added alchlor when adjusting pH value=7.5-8.0, obtains Lithol Red.
2. a kind of preparation method of Lithol Red according to claim 1, which is characterized in that the anionic surface is living
Property agent be one of turkey red oil, sodium alkyl benzene sulfonate, stearic acid or a variety of.
3. a kind of preparation method of Lithol Red according to claim 2, which is characterized in that the anionic surface is living
Property agent be turkey red oil.
4. a kind of preparation method of Lithol Red according to claim 1, which is characterized in that the quality of the hydrochloric acid point
Number is 24-26%.
5. a kind of preparation method of Lithol Red according to claim 4, which is characterized in that the quality of the liquid alkaline point
Number is 25-28%.
6. a kind of preparation method of Lithol Red according to claim 1, which is characterized in that idol described in step (1)
The temperature for closing liquid is 15-20 DEG C.
7. a kind of preparation method of Lithol Red according to claim 1, which is characterized in that pine described in step (3)
The temperature of perfume dissolution is 90-95 DEG C.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102399453A (en) * | 2010-09-14 | 2012-04-04 | 南通锦悦服装设计有限公司 | Preparation method of fast scarlet 48:1 organic pigment |
| CN102838883A (en) * | 2012-09-25 | 2012-12-26 | 山东宇虹新颜料股份有限公司 | Preparation method for C.I. paratonere 49:1 |
-
2018
- 2018-11-20 CN CN201811382489.8A patent/CN109370249A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102399453A (en) * | 2010-09-14 | 2012-04-04 | 南通锦悦服装设计有限公司 | Preparation method of fast scarlet 48:1 organic pigment |
| CN102838883A (en) * | 2012-09-25 | 2012-12-26 | 山东宇虹新颜料股份有限公司 | Preparation method for C.I. paratonere 49:1 |
Non-Patent Citations (1)
| Title |
|---|
| JENS STENGER ET AL.: "Lithol red salts: characterization and deteriorationage/", 《E-PRESERVATION SCIENCE》 * |
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