CN107573721A - A kind of permanent bordeaux pigment and preparation method thereof - Google Patents
A kind of permanent bordeaux pigment and preparation method thereof Download PDFInfo
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- CN107573721A CN107573721A CN201711001216.XA CN201711001216A CN107573721A CN 107573721 A CN107573721 A CN 107573721A CN 201711001216 A CN201711001216 A CN 201711001216A CN 107573721 A CN107573721 A CN 107573721A
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Abstract
The invention belongs to method for preparing pigment technical field, more particularly to a kind of permanent bordeaux pigment and preparation method thereof, including following each component by weight：Large red-based g：2%‑4%；Hydrochloric acid：4%‑6%；Natrium nitrosum：1%‑3%；Sulfamic acid：0.1%‑1%；Azoic coupling component AS：4%‑7%；Liquid caustic soda：2%‑5%；Sodium acetate：0.5%‑2%；Flake ice：20%‑25%；Water：58% 65%, and a kind of preparation method of permanent bordeaux pigment.The present invention prepares the good permanent bordeaux pigment of using effect, the present invention has preparation method easy and prepares the advantages of pigment using effect of gained is good by the control of each composition proportion of permanent bordeaux pigment and method technique.
Description
Technical field
The invention belongs to method for preparing pigment technical field, more particularly to a kind of permanent bordeaux pigment and preparation method thereof.
Background technology
China is not only the big producer of organic pigment at present, while is increasingly becoming the use big country of organic pigment, face
Material has enter into the every field of people's life, and multicoloured color has brought endless joy.With material and
The development of spiritual civilization, it is environmentally friendly the problem of it is more and more important, the problem of to there has been proposed how to preserve the ecological environment, for having
The safety issue of machine pigment, European Union promulgated REACH regulations, it is specified that organic pigment prohibits the use of first on June 1st, 2007
24 kinds of aromatic amines with carcinogenicity, eight big harmful heavy metal contents can not be exceeded.Required according to this, during we live
The textile used, such as most of art ticking, quilt cover do not meet environmental requirement, and foreign countries emphasize low stainization and reach high
Two target bindings of performance, in order to improve the ecological environment, open up the international market of organic pigment, organic pigment is also necessary
Meet the requirement of environmental protection.
The Chinese invention patent that patent application publication number is the A of CN 105062197, data of publication of application is 2015.11.18 is public
A kind of environmental-friendly nitryl ink permanent bordeaux composite pigment and preparation method thereof is opened, by the component system for including following parts by weight
Into：Permanent bordeaux 2BL2-4 parts, polyethylene glycol diamines 15-25 parts, acetone 11-20 parts, zinc oxide 5-11 parts, paraffin oil 5-9 parts, receive
Rice silica 3-6 parts, butyl acetate 2-3 parts, ammonium persulfate 1-3 parts, IPD 0.5-1 parts and benzoyl peroxide
0.5-1 parts, the invention additionally provide a kind of preparation method of environmental-friendly nitryl ink permanent bordeaux composite pigment.But the invention
Pigment in patent has using effect poor, and preparation method has the problem of technique is complicated.
The content of the invention
It is an object of the invention to provide a kind of permanent bordeaux pigment and preparation method thereof, and it can pass through each composition of permanent bordeaux pigment
The control of proportioning and method technique, the good permanent bordeaux pigment of using effect is prepared, the present invention has preparation method easy and system
The advantages of pigment using effect of standby gained is good.
The solve the above problems technical scheme of use of the present invention is：A kind of permanent bordeaux pigment, including by weight following
Each component：Large red-based g：2%-4%；Hydrochloric acid：4%-6%；Natrium nitrosum：1%-3%；Sulfamic acid：0.1%-1%；Azoic coupling component AS：4%-
7%；Liquid caustic soda：2%-5%；Sodium acetate：0.5%-2%；Flake ice：20%-25%；Water：58%-65%.
Further preferred technical scheme is：The hydrochloric acid mass fraction is 30%.
Further preferred technical scheme is：The liquid caustic soda mass fraction is 20%-35%, solute be sodium hydroxide and
Potassium hydroxide.
Further preferred technical scheme is：Active ingredient 2- amino -4- nitrotoleunes in the large red-based g
Mass fraction be 78%-85%.
Further preferred technical scheme is：The natrium nitrosum, sulfamic acid, the purity of azoic coupling component AS and sodium acetate
As mass fraction, purity range 98%-100%.
A kind of preparation method of permanent bordeaux pigment, comprises the following steps：
（1）In sour environment, large red-based g solution, flake ice and sodium nitrite solution are sequentially added, it is anti-that diazotising occurs
Should, and sulfamic acid solution is added after abundant reaction, diazo liquid is made；
（2）Azoic coupling component AS solution, flake ice and sodium acetate solution are sequentially added in water, coupling solution is made after being sufficiently stirred；
（3）Coupling solution is first held in coupling bucket, then diazo liquid is added dropwise, after multiple stirring and pH regulation operations, heating
Simultaneously press filtration is stood, obtains pigment product.
Further preferred technical scheme is：Step（1）In, sour environment includes the hydrochloric acid of 30% parts by weight, adds big
Stirred after red base G solution and be cooled to 0-3 DEG C by adding flake ice, add sodium nitrite solution, diazo-reaction occurs,
After question response system to alkalescence, stir and add sulfamic acid solution, diazo liquid is made.
Further preferred technical scheme is：Step（2）In, azoic coupling component AS solution includes the liquid caustic soda of 30% parts by weight, color
Phenol AS solution by adding flake ice is cooled to 15-18 DEG C after being completely dissolved, then is added by way of being slowly added dropwise, quickly stirring
Sodium acetate solution, finally it is slowly stirred again after all adding, coupling solution is made.
Further preferred technical scheme is：Step（3）In, diazo liquid is added dropwise for the first time into coupling solution so that pH
Near 4.1-4.4, liquid caustic soda is added, adjust pH to 5.5-5.9, second of dropwise addition diazo liquid, until pH returns 4.1-4.4 models
Enclose, coupling reaction finishes, and finally carries out pH regulations and heating temperature control operation.
Further preferred technical scheme is：Step（3）In, stir and be rapidly heated to 60- after coupling reaction
65 DEG C, it is incubated and adjusts pH to 9.0-9.5, stood after stirring, treat press filtration to obtain pigment product.
The present invention prepares the good permanent bordeaux of using effect by the control of each composition proportion of permanent bordeaux pigment and method technique
Pigment, the present invention have preparation method easy and prepare the advantages of pigment using effect of gained is good.
Embodiment
As described below is only presently preferred embodiments of the present invention, non-that the scope of the present invention is defined.
Embodiment 1
A kind of permanent bordeaux pigment and preparation method thereof, comprises the following steps：
（1）5000kg water is first added in diazonium bucket and 1350kg mass fractions are 30% hydrochloric acid, and is stirred, then is added
Enter large red-based g solution（2000kg water+980kg large red-based gs, are pre-configured with）, and be stirred, then add 3300kg pieces
Ice adjusts temperature of reaction system to 1 DEG C, and sodium nitrite solution is slowly added dropwise in 2h time again after temperature stabilization（2000kg water
+ 450kg natrium nitrosums, are pre-configured with）, stirred when being added dropwise, to carry out diazo-reaction, repeatedly measure pH test paper as blueness,
I.e. pH stable is in 10 or so rear addition sulfamic acid solutions（1000kg water+80kg sulfamic acids, are pre-configured with）, diazotising is anti-
It should terminate；
（2）5000kg water and azoic coupling component AS solution are first added in dissolving bucket（1800kg water+200kg mass fractions are 30% hydrogen
Sodium hydroxide solution+1200kg azoic coupling component AS, are pre-configured with）, stirring and dissolving 8-10h is until be completely dissolved, then be all added to coupling
In bucket, and flake ice 4000kg is added, be cooled to 15 DEG C, then add sodium acetate solution（2200kg water+200kg sodium acetates, in advance
Configuration）And controlling to be slowly added dropwise in 35min and finish, dropwise addition process is quickly stirred, and 10min is slowly stirred after completion of dropwise addition,
Coupling solution is prepared and finished；
（3）By diazo liquid be slowly added into coupling bucket in, to pH be 4.2 when stop add, change plus mass fraction be 30% hydrogen-oxygen
Change sodium, until pH is adjusted to 5.7, then diazo liquid is added dropwise again until pH is returned to 4.2, the present invention time is 5h, the above
Complete whole coupling reaction；
（4）To step（3）In obtained pigment crude product be stirred heating, to 60 DEG C, and be incubated 1.5h, be with mass fraction
30% sodium hydroxide regulation pH to 9.2, the stirring and 2h for finally carrying out 10min are stood, and pigment product is obtained by filter press.
In the present embodiment, diazo liquid preparation, coupling solution preparation and the step of coupling reaction three are passed sequentially through to be made forever solid
Red so that the present invention has the advantages of preparation method is simple and efficient.To the pigment product finally obtained in the present embodiment, just
Four fineness, weatherability, light resistance and solvent resistance aspects are tested and analyzed, and record result to make comparisons.
Embodiment 2
A kind of permanent bordeaux pigment and preparation method thereof, comprises the following steps：
（1）4800kg water is first added in diazonium bucket and 1250kg mass fractions are 30% hydrochloric acid, and is stirred, then is added
Enter large red-based g solution（2000kg water+950kg large red-based gs, are pre-configured with）, and be stirred, then add 3200kg pieces
Ice adjusts temperature of reaction system to 2 DEG C, and sodium nitrite solution is slowly added dropwise in 2h time again after temperature stabilization（2000kg water
+ 420kg natrium nitrosums, are pre-configured with）, stirred when being added dropwise, to carry out diazo-reaction, repeatedly measure pH test paper as blueness,
I.e. pH stable is in 10 or so rear addition sulfamic acid solutions（1000kg water+75kg sulfamic acids, are pre-configured with）, diazotising is anti-
It should terminate；
（2）4800kg water and azoic coupling component AS solution are first added in dissolving bucket（1700kg water+180kg mass fractions are 30% hydrogen
Sodium hydroxide solution+1100kg azoic coupling component AS, are pre-configured with）, stirring and dissolving 8-10h is until be completely dissolved, then be all added to coupling
In bucket, and flake ice 3900kg is added, be cooled to 16 DEG C, then add sodium acetate solution（2200kg water+190kg sodium acetates, in advance
Configuration）And controlling to be slowly added dropwise in 35min and finish, dropwise addition process is quickly stirred, and 10min is slowly stirred after completion of dropwise addition,
Coupling solution is prepared and finished；
（3）By diazo liquid be slowly added into coupling bucket in, to pH be 4.3 when stop add, change plus mass fraction be 30% hydrogen-oxygen
Change sodium, until pH is adjusted to 5.8, then diazo liquid is added dropwise again until pH is returned to 4.3, the present invention time is 5h, the above
Complete whole coupling reaction；
（4）To step（3）In obtained pigment crude product be stirred heating, to 60 DEG C, and be incubated 1.5h, be with mass fraction
30% sodium hydroxide regulation pH to 9.3, the stirring and 2h for finally carrying out 10min are stood, and pigment product is obtained by filter press.
In the present embodiment, diazo liquid preparation, coupling solution preparation and the step of coupling reaction three are passed sequentially through to be made forever solid
Red so that the present invention has the advantages of preparation method is simple and efficient.To the pigment product finally obtained in the present embodiment, just
Four fineness, weatherability, light resistance and solvent resistance aspects are tested and analyzed, and record result to make comparisons.
Embodiment 3
A kind of permanent bordeaux pigment and preparation method thereof, comprises the following steps：
（1）5200kg water is first added in diazonium bucket and 1450kg mass fractions are 30% hydrochloric acid, and is stirred, then is added
Enter large red-based g solution（2000kg water+1000kg large red-based gs, are pre-configured with）, and be stirred, then add 3400kg
Flake ice adjusts temperature of reaction system to 3 DEG C, and sodium nitrite solution is slowly added dropwise in 2h time again after temperature stabilization（2000kg
Water+480kg natrium nitrosums, are pre-configured with）, stirred when being added dropwise, to carry out diazo-reaction, repeatedly measure pH test paper as indigo plant
Color, i.e. pH stable are in 10 or so rear addition sulfamic acid solutions（1000kg water+90kg sulfamic acids, are pre-configured with）, diazonium
Change reaction to terminate；
（2）5200kg water and azoic coupling component AS solution are first added in dissolving bucket（1900kg water+210kg mass fractions are 30% hydrogen
Sodium hydroxide solution+1300kg azoic coupling component AS, are pre-configured with）, stirring and dissolving 8-10h is until be completely dissolved, then be all added to coupling
In bucket, and flake ice 4200kg is added, be cooled to 16 DEG C, then add sodium acetate solution（2200kg water+210kg sodium acetates, in advance
Configuration）And controlling to be slowly added dropwise in 35min and finish, dropwise addition process is quickly stirred, and 10min is slowly stirred after completion of dropwise addition,
Coupling solution is prepared and finished；
（3）By diazo liquid be slowly added into coupling bucket in, to pH be 4.3 when stop add, change plus mass fraction be 30% hydrogen-oxygen
Change sodium, until pH is adjusted to 5.8, then diazo liquid is added dropwise again until pH is returned to 4.3, the present invention time is 5h, the above
Complete whole coupling reaction；
（4）To step（3）In obtained pigment crude product be stirred heating, to 60 DEG C, and be incubated 1.5h, be with mass fraction
30% sodium hydroxide regulation pH to 9.3, the stirring and 2h for finally carrying out 10min are stood, and pigment product is obtained by filter press.
In the present embodiment, diazo liquid preparation, coupling solution preparation and the step of coupling reaction three are passed sequentially through to be made forever solid
Red so that the present invention has the advantages of preparation method is simple and efficient.To the pigment product finally obtained in the present embodiment, just
Four fineness, weatherability, light resistance and solvent resistance aspects are tested and analyzed, and record result to make comparisons.
By detection and analysis the result record such as following table of above-mentioned 3 embodiments：
| Sequence number | Fineness | Weatherability | Light resistance | Solvent resistance |
| Embodiment 1 | <3μm | 5 | 8 grades | 5 grades |
| Embodiment 2 | <4μm | 5 | 8 grades | 5 grades |
| Embodiment 3 | <3μm | 4 | 8 grades | 5 grades |
As can be seen from the above table, embodiment 1-3 is less than 4 μm in terms of pigment fineness, preferably can be met after various
Requirement in continuous technique, and weatherability, light resistance and solvent resistance are also in high grade, can be as comparing
It is that weatherability is more than or equal to 4, light resistance and is more than or more than 7 grades and solvent resistance is general more than or equal to 4 grades of pigment all
Fine efficient, the lasting class pigment of preservation is identified as, suitable for most of dyeing.
In addition, in the present invention, the addition of liquid caustic soda, flake ice and water is using mode is added portionwise, for different phase
Or not same-action, but its total amount meets the component proportion of permanent bordeaux pigment.
Embodiments of the present invention are explained in detail above, but the invention is not restricted to above-mentioned embodiment, in institute
State in technical field those of ordinary skill's possessed knowledge, can also be made on the premise of present inventive concept is not departed from
Various modifications.These are all without creative modification, as long as all by Patent Law in scope of the presently claimed invention
Protection.
Claims (10)
1. a kind of permanent bordeaux pigment, it is characterised in that including following each component by weight：Large red-based g：2%-4%；Salt
Acid：4%-6%；Natrium nitrosum：1%-3%；Sulfamic acid：0.1%-1%；Azoic coupling component AS：4%-7%；Liquid caustic soda：2%-5%；Sodium acetate：0.5%-
2%；Flake ice：20%-25%；Water：58%-65%.
A kind of 2. permanent bordeaux pigment according to claim 1, it is characterised in that：The hydrochloric acid mass fraction is 30%.
A kind of 3. permanent bordeaux pigment according to claim 1, it is characterised in that：The liquid caustic soda mass fraction is 20%-35%,
Solute is sodium hydroxide and potassium hydroxide.
A kind of 4. permanent bordeaux pigment according to claim 1, it is characterised in that：Active ingredient 2- in the large red-based g
The mass fraction of amino -4- nitrotoleunes is 78%-85%.
A kind of 5. permanent bordeaux pigment according to claim 1, it is characterised in that：The natrium nitrosum, sulfamic acid, azoic coupling component
The purity of AS and sodium acetate as mass fraction, purity range 98%-100%.
A kind of 6. preparation method of the permanent bordeaux pigment in 1-5 such as claim as described in any one, it is characterised in that including with
Lower step：
（1）In sour environment, large red-based g solution, flake ice and sodium nitrite solution are sequentially added, it is anti-that diazotising occurs
Should, and sulfamic acid solution is added after abundant reaction, diazo liquid is made；
（2）Azoic coupling component AS solution, flake ice and sodium acetate solution are sequentially added in water, coupling solution is made after being sufficiently stirred；
（3）Coupling solution is first held in coupling bucket, then diazo liquid is added dropwise, after multiple stirring and pH regulation operations, heating
Simultaneously press filtration is stood, obtains pigment product.
A kind of 7. preparation method of permanent bordeaux pigment according to claim 6, it is characterised in that：Step（1）In, acyclic acidic
Border includes the hydrochloric acid of 30% parts by weight, is stirred after adding large red-based g solution and is cooled to 0-3 DEG C by adding flake ice, added
Sodium nitrite solution, diazo-reaction occurs, after question response system to alkalescence, stir and add sulfamic acid solution, weight is made
Nitrogen liquid.
A kind of 8. preparation method of permanent bordeaux pigment according to claim 6, it is characterised in that：Step（2）In, azoic coupling component AS
Solution includes the liquid caustic soda of 30% parts by weight, and azoic coupling component AS solution by adding flake ice is cooled to 15-18 DEG C after being completely dissolved, then leads to
Cross be slowly added dropwise, the mode that quickly stirs adds sodium acetate solution, finally is slowly stirred again after all adding, be made and be coupled
Liquid.
A kind of 9. preparation method of permanent bordeaux pigment according to claim 6, it is characterised in that：Step（3）In, toward coupling
Diazo liquid is added dropwise in liquid for the first time so that the near 4.1-4.4 of pH, add liquid caustic soda, adjust pH to 5.5-5.9, second of dropwise addition
Diazo liquid, until pH returns 4.1-4.4 scopes, coupling reaction finishes, and finally carries out pH regulations and heating temperature control operation.
A kind of 10. preparation method of permanent bordeaux pigment according to claim 9, it is characterised in that：Step（3）In, coupling
Stir and be rapidly heated to 60-65 DEG C after completion of the reaction, be incubated and adjust pH to 9.0-9.5, stood after stirring, treat press filtration to obtain
Obtain pigment product.
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| CN201711001216.XA CN107573721A (en) | 2017-10-24 | 2017-10-24 | A kind of permanent bordeaux pigment and preparation method thereof |
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| CN201711001216.XA CN107573721A (en) | 2017-10-24 | 2017-10-24 | A kind of permanent bordeaux pigment and preparation method thereof |
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