CN108587250A - A kind of composite pigment surface modifier and its application process - Google Patents
A kind of composite pigment surface modifier and its application process Download PDFInfo
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- CN108587250A CN108587250A CN201710675818.7A CN201710675818A CN108587250A CN 108587250 A CN108587250 A CN 108587250A CN 201710675818 A CN201710675818 A CN 201710675818A CN 108587250 A CN108587250 A CN 108587250A
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- pigment
- surfactant
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- surface modifier
- active agent
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
- C09C1/56—Treatment of carbon black ; Purification
-
- 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
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0001—Post-treatment of organic pigments or dyes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
-
- 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
- C09D17/00—Pigment pastes, e.g. for mixing in paints
- C09D17/001—Pigment pastes, e.g. for mixing in paints in aqueous medium
-
- 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
- C09D17/00—Pigment pastes, e.g. for mixing in paints
- C09D17/003—Pigment pastes, e.g. for mixing in paints containing an organic 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
- C09D17/00—Pigment pastes, e.g. for mixing in paints
- C09D17/004—Pigment pastes, e.g. for mixing in paints containing an inorganic pigment
- C09D17/005—Carbon black
Abstract
The invention discloses a kind of composite pigment surface modifier and its application processes, belong to technical field of fine.Anionic surfactant and nonionic surface active agent is used to compound as compound surface-treating agent present invention is disclosed a kind of, and using the compound surface-treating agent to the method for pigment progress surface modification, modified pigment is used to prepare aqueous color paste, and dispersion effect, stability and tinting strength, tinting power are significantly improved.
Description
Technical field
The invention belongs to the technical fields of fine chemistry industry, more particularly, it relates to which a kind of composite pigment surface changes
Property agent and its application process, aqueous color paste prepared by modified pigment has in the performances such as dispersion effect, stability and tinting strength, tinting power
It significantly improves.
Background technology
By carrying out surface modification to pigment, changes the physical and chemical performance of pigment particle surface, be pigment processing and manufacturing
Field promotes the common method of pigment added value and using effect.
In order to avoid directly using caused dust pollution, serious, the excessive caused tinting strength, tinting power of granules of pigments drops powder pigment
Low, the problems such as metering is inconvenient, granules of pigments is stably dispersed in the aqueous color paste formed in water-based system, is to obtain in recent years
Widely applied novel colorant.Aqueous color paste be usually by powder pigment in the water-based system containing dispersant through overmulling
Close, grinding, dispersion etc. techniques be prepared, by surface of pigments modification technology reduce mill base in granules of pigments particle diameter distribution,
Its tinting strength, tinting power and stability are promoted, is the hot spot of pigment manufacture field research in recent years.
Application No. is the Chinese patent of CN201210063948.2, discloses a kind of aromatic series phosphorus-containing compound and contain with alkyl
The method that phosphorus compound is surface-treated pigment, treated when pigment is used to prepare aqueous color paste stability and tinting strength, tinting power
It is significantly improved, but during pigment use, it is difficult to avoiding phosphorus-containing compound from being discharged into water can cause water body richness to seek
Fosterization;The United States Patent (USP) of Publication No. US6120596 discloses a kind of halogen-containing silane compound of use to pigment carry out table
The method that face is modified, this method can promote dispersion effect of the granules of pigments in mill base, reduce particle diameter distribution, but this method institute
With halogen-containing silane compound, expensive and dosage is larger, and pigment modification cost is higher.
The completion surface of pigments modification of low cost promotes dispersion effect, stability and coloring of the granules of pigments in mill base
Power, be develop high-performance, inexpensive dispersible pigment color paste important channel.
Invention content
Technical problems based on background technology, present invention aims at provide a kind of composite pigment surface modifier
And its application process;This method is by using specific anionic surfactant and nonionic surface active agent compounding pair
Pigment carries out surface modification, and mill base prepared by modified pigment, dispersion effect, stability and tinting strength, tinting power are significantly improved.
A kind of composite pigment surface modifier composite pigment surface modifier includes following component:It lives on anionic surface
Property agent and nonionic surface active agent, and the anionic surfactant is the compound with general formula (I) structure:
Wherein, n is the integer between 1~500, and includes 1 and 500;
The nonionic surface active agent is the compound with general formula (II) structure,
Wherein, R1And R2It is the alkyl or aromatic radical containing carbon number between 3~10, and includes 3 and 10, R3And R4It is H, first
One kind in base, ethyl, R5And R6It is one kind in H, methyl, the sum of p and q are the integers between 1~30, and include 1 and 30.
In the present invention, anionic surfactant used is benzene sulfonic acid sodium salt class surfactant, nonionic table used
Face activating agent is acetylenic diols surfactant.
In the present invention, the n in anionic surfactant general formula (I) structure used is preferably 5~50.Nonionic used
Type surfactant general formula (II) structure R5And R6For H, which is acetylenic diols surfactant, alkynes
Containing amphiphilic structure, hydrophobic grouping in glycols surfactant molecule, triple carbon-carbon bonds, ethyoxyl and hydroxyl all have polarity,
The ratio of ethyoxyl number different structure difference or hydrophobic group/hydrophilic radical in molecule is different, then can obtain different parents
The acetylenic diols surfactant of the surfactant of hydrophile-lipophile balance value, general formula (II) structure can be by acetylenic glycols to epoxy second
Alkane/propylene oxide open loop addition and obtain.
Disclosed composite pigment surface modifier application process, applying step are as follows:
Step 1:It is prepared by surfactant mixed liquor:Anionic surfactant, nonionic surface active agent is molten
In solution to water, it is 9.0-11.0 to adjust pH value using alkaline pH adjuster, obtains mixed solution, anionic surface activity
The mass ratio of agent, nonionic surface active agent and deionized water is 5~25:1~3:1000;
Step 2:The preparation of graining paste:It is 40-85 DEG C, under stirring in temperature, the step 1 is added in pigment and is made
Mixed solution in, it is agitated, grind, graining paste is obtained by filtration, wherein the matter of pigment used and deionized water used in step 1
Amount is than being 100~300:1000;The grinding is ground using horizontal sand mill or ball mill;
Step 3:By the spray-dried machine drying of graining paste and granulation obtained by step 2, the modified pigment in surface is obtained
Particle.
Wherein, the alkaline pH adjuster in step 1 is sodium hydroxide, ammonium hydroxide, sodium bicarbonate, sodium dihydrogen phosphate, acetic acid
At least one of sodium, triethanolamine.
The modified granules of pigments in surface obtained, the application in preparing aqueous color paste.
In pigment production and application field, pigment product call number may be used to indicate the concrete structure of pigment, such as benzene
And imidazolone Huang is named as C.I. pigment yellow 154s, phthalocyanine blue 15:3 pigment are named as C.I. pigment blue 15s:3, organic pigment
The concrete structure of pigment representated by product call number can according to organic pigment product call number from《Organic pigment index card》Deng often
It is inquired in books.
In the present invention, to pigment used, there is no particular restriction, and pigment used can be but not limited to following pigment:Carbon black,
C.I. pigment red 48: 2, C.I. pigment red 4s 8: 4, C.I. pigment red 4s 9: 1, C.I. paratoneres 52: 2, C.I. paratoneres 64: 1,
C.I. pigment red 81, C.I. pigment Red 8s 8, C.I. Pigment Red 9s 2, C.I. paratoneres 101, C.I. pigment Yellow 14s, C.I. pigment yellows
74, C.I. pigment yellows 95, C.I. pigment yellows 100, C.I. pigment blue 15s: 3, C.I. pigment blue 15s: 4, C.I. pigment blue 15s: 6,
C.I. pigment blue 17: 1, C.I. pigment blues 56, C.I. pigment blues 63.
Surface-modified pigments made from disclosed composite pigment surface modifier and its application process, it is main to use
In preparing aqueous color paste.Compared with prior art, the device have the advantages that being:
The present invention by after anionic surfactant and nonionic surface active agent are compounded to pigment into
Row surface is modified, and aqueous color paste prepared by modified pigment, dispersion effect, stability and tinting strength, tinting power are significantly improved.
Specific implementation mode
Below by embodiment, comparative example and Application Example, the outstanding advantages and show that the present invention is further explained
Work feature, but the present invention is not limited to the following example and Application Example.
The present invention is made further to explain with reference to specific embodiment.
In the following example, comparative example and Application Example, anionic surfactant A used1、A2、A3Have
There is the structure of general formula (I):
Wherein A1In, n 5;A2In, n 50;A3In, n 30.
Nonionic surface active agent B used1、B2、B3All have the structure of general formula (II):
Wherein, B1In, R1And R2It is propyl, R3And R4It is ethyl, R5And R6It is methyl, p and q is 8;B2In, R1
And R2It is phenyl, R3And R4It is methyl, R5And R6Be H, p and q it is 12;B3In, R1And R2It is decyl, R3And R4
For H, R5And R6Be H, p and q it is 30.
Embodiment 1
2.5g anionic surfactant A1,1.5g nonionic surface active agent B1 is dissolved into 500g water, is used
The pH value that 20wt.%NaOH aqueous solutions adjust the slurry is 11.0, in the case where temperature is 85 DEG C, mixing speed is 500r/min,
50g carbon blacks are added in mixed solution, after continuing stirring 1 hour, mixed slurry are ground 3 times through sand mill, through filtering
To graining paste, the graining paste that will be obtained, spray-dried machine is dry and granulation obtains the modified granules of pigments in surface.
Embodiment 2
12.5g anionic surfactant A1,0.5g nonionic surface active agent B2 is dissolved into 500g water, is used
The pH value that 15wt.% ammonia spirits adjust the slurry is 9.0, will in the case where temperature is 40 DEG C, mixing speed is 1000r/min
100g paratoneres 254 are added in mixed solution, after continuing stirring 3 hours, by mixed slurry through ball mill grinding 20 minutes, warp
Graining paste is obtained by filtration, the graining paste that will be obtained, spray-dried machine is dry and granulation obtains the modified granules of pigments in surface.
Embodiment 3
5g anionic surfactant A2,1g nonionic surface active agent B1 is dissolved into 500g water, is used
The pH value that 15wt.% ammonia spirits adjust the slurry is 9.0, will in the case where temperature is 60 DEG C, mixing speed is 1000r/min
100g pigment blue 15s:0 is added in mixed solution, after continuing stirring 3 hours, by mixed slurry through ball mill grinding 30 minutes,
Through graining paste is obtained by filtration, the graining paste that will be obtained, spray-dried machine is dry and granulation obtains the modified pigment in surface
Grain.
Embodiment 4
10g anionic surfactant A3,1.2g nonionic surface active agent B3 is dissolved into 500g water, is used
It is 10.0 that 30wt.%KOH aqueous solutions, which adjust pH value, in the case where temperature is 75 DEG C, mixing speed is 1500r/min, by 150g pigment
Red 254 are added in mixed solution, after continuing stirring 1 hour, mixed slurry are ground 5 times through sand mill, through face is obtained by filtration
Slurry, the graining paste that will be obtained, spray-dried machine is dry and granulation obtains the modified granules of pigments in surface.
Comparative example 5
2.5g anionic surfactant A1 is dissolved into 500g water, described in the adjusting of 20wt.%NaOH aqueous solutions
The pH value of slurry is 11.0, and in the case where temperature is 85 DEG C, mixing speed is 500r/min, 50g carbon blacks are added in mixed solution,
After continuing stirring 1 hour, mixed slurry is ground 3 times through sand mill, through graining paste is obtained by filtration, the graining paste that will be obtained, warp
Spray dryer is dry and granulation obtains the modified granules of pigments in surface.
Comparative example 6
1.5g nonionic surface active agent B2 is dissolved into 500g water, described in the adjusting of 20wt.%NaOH aqueous solutions
The pH value of slurry is 11.0, and in the case where temperature is 85 DEG C, mixing speed is 500r/min, 50g carbon blacks are added in mixed solution,
After continuing stirring 1 hour, mixed slurry is ground 3 times through sand mill, through graining paste is obtained by filtration, the graining paste that will be obtained, warp
Spray dryer is dry and granulation obtains the modified granules of pigments in surface.
Comparative example 7
5g anionic surfactant neopelex, 1g nonionic surface active agent B1 are dissolved into
In 500g water, the pH value that the slurry is adjusted with 15wt.% ammonia spirits is 9.0, temperature is 60 DEG C, mixing speed is
Under 1000r/min, by 100g pigment blue 15s:0 is added in mixed solution, after continuing stirring 3 hours, by mixed slurry through ball milling
Machine is ground 30 minutes, and through graining paste is obtained by filtration, the graining paste that will be obtained, spray-dried machine is dry and is granulated to change to surface
Granules of pigments after property.
Comparative example 8
6g anionic surfactant A2 is dissolved into 1000g water, the slurry is adjusted with 15wt.% ammonia spirits
PH value be 9.0, in the case where temperature is 60 DEG C, mixing speed is 1000r/min, by 100g pigment blue 15s:0 is added to mixed solution
In, after continuing stirring 3 hours, by mixed slurry through ball mill grinding 30 minutes, through graining paste is obtained by filtration, the pigment that will obtain
Slurry, spray-dried machine is dry and granulation obtains the modified granules of pigments in surface.
Application Example 9~16
Following Application Example 9-16 is implemented with formula composition listed by table 1 using unmodified pigment and through embodiment, comparison
Aqueous color paste is prepared through mixing, dispersion, grinding, defoaming in the modified pigment of example, and it is total to be that each component accounts for mill base for data in table
The mass percent of quality.
Composition (the unit of 1. Application Example 9-16 of table:Mass percent)
Dispersion effect is tested:It is real with the MS2000 laser micron grain size instrument test application of Malvern Instr Ltd. of Britain
Apply a particle diameter distribution for aqueous color paste prepared by 9-16, in test result, D50 indicates that in surveyed particle 50% particle can lead to
The minimum grain size crossed can relatively accurately judge that dispersion of the different pigment in mill base is imitated by the particle diameter distribution D50 of pigment
Fruit.
Stability test:Aqueous color paste prepared by Application Example 9-16 at 25 DEG C distinguish it is closed place 90 days and
After 180 days, by visual observations, whether there is or not the case where apparent granules of pigments precipitation, flocculation etc. seriously affect stability occur to judge
The storage stability of aqueous color paste.
Tinting strength, tinting power is tested:According to B methods (instrumental method) test application embodiment 9- described in HG/T 3951-2007 Appendix B
16 relative color strength, wherein Application Example 9-12 are using 9 made mill base of Application Example as standard mill base, Application Example
13-16 is using 13 made mill base of Application Example as standard mill base.
Table 2 is the result that aqueous color paste prepared by Application Example 9-16 is tested according to the above method.Wherein stable storing
Property test in, " √ " indicates that range estimation is without exception, and "×" indicates that situations such as apparent granules of pigments precipitation, flocculation occurs in range estimation.
Aqueous color paste the performance test results prepared by 2. Application Example 9-16 of table
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (8)
1. a kind of composite pigment surface modifier, which is characterized in that the composite pigment surface modifier includes following component:The moon from
Subtype surfactant and nonionic surface active agent,
The anionic surfactant is the compound with general formula (I) structure:
Wherein, n is the integer between 1~500, and includes 1 and 500;
The nonionic surface active agent is the compound with general formula (II) structure,
Wherein, R1And R2It is the alkyl or aromatic radical containing carbon number between 3~10, and includes 3 and 10, R3And R4It is H, methyl, second
One kind in base, R5And R6It is one kind in H, methyl, the sum of p and q are the integers between 1~30, and include 1 and 30.
2. composite pigment surface modifier according to claim 1, it is characterised in that:The anionic surfactant
For benzene sulfonic acid sodium salt class surfactant.
3. composite pigment surface modifier according to claim 1, it is characterised in that:The nonionic surface active agent
For acetylenic diols surfactant.
4. composite pigment surface modifier according to claim 1, it is characterised in that:The anionic surfactant
N in general formula (I) structure is 5~50.
5. composite pigment surface modifier according to claim 1, it is characterised in that:The nonionic surface active agent
General formula (II) structure R5And R6For H.
6. a kind of composite pigment surface modifier application process, it is characterised in that:Its applying step is as follows:
Step 1:It is prepared by surfactant mixed liquor:Anionic surfactant, nonionic surface active agent are dissolved into
In water, it is 9.0-11.0 to adjust pH value using alkaline pH adjuster, obtains mixed solution, anionic surfactant, non-
Ionic surfactant and the mass ratio of deionized water are 5~25:1~3:1000;
Step 2:The preparation of graining paste:It is 40-85 DEG C, under stirring in temperature, pigment is added made from the step 1 and is mixed
It closes in solution, it is agitated, grind, graining paste is obtained by filtration, wherein the mass ratio of pigment used and deionized water used in step 1
It is 100~300:1000;The grinding is ground using horizontal sand mill or ball mill;
Step 3:By the spray-dried machine drying of graining paste and granulation obtained by step 2, the modified granules of pigments in surface is obtained.
7. a kind of preparation method of pigment modification agent according to claim 6, it is characterised in that:Alkali in the step 1
Property pH adjusting agent be sodium hydroxide, ammonium hydroxide, sodium bicarbonate, sodium dihydrogen phosphate, sodium acetate, at least one of triethanolamine.
8. power will require the granules of pigments that surface is modified made from 6 preparation methods, the application in preparing aqueous color paste.
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CN112812615A (en) * | 2021-01-27 | 2021-05-18 | 宇虹颜料股份有限公司 | Preparation method of graphene-containing easily-dispersible pigment |
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JP2006219584A (en) * | 2005-02-10 | 2006-08-24 | Seiko Epson Corp | Water-based carbon black dispersion, method for producing the same and water-based ink |
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CN112812615A (en) * | 2021-01-27 | 2021-05-18 | 宇虹颜料股份有限公司 | Preparation method of graphene-containing easily-dispersible pigment |
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