CN109385116A - A kind of permanent bordeaux pigment and preparation method thereof with strong dispersibility - Google Patents

A kind of permanent bordeaux pigment and preparation method thereof with strong dispersibility Download PDF

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Publication number
CN109385116A
CN109385116A CN201811397605.3A CN201811397605A CN109385116A CN 109385116 A CN109385116 A CN 109385116A CN 201811397605 A CN201811397605 A CN 201811397605A CN 109385116 A CN109385116 A CN 109385116A
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CN
China
Prior art keywords
parts
added
pigment
preparation
permanent bordeaux
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CN201811397605.3A
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Chinese (zh)
Inventor
龚国平
叶连喜
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Xuancheng Inter Pigment Co Ltd
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Xuancheng Inter Pigment Co Ltd
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Priority to CN201811397605.3A priority Critical patent/CN109385116A/en
Publication of CN109385116A publication Critical patent/CN109385116A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B29/00Monoazo dyes prepared by diazotising and coupling
    • C09B29/10Monoazo dyes prepared by diazotising and coupling from coupling components containing hydroxy as the only directing group
    • C09B29/18Monoazo dyes prepared by diazotising and coupling from coupling components containing hydroxy as the only directing group ortho-Hydroxy carbonamides
    • C09B29/20Monoazo dyes prepared by diazotising and coupling from coupling components containing hydroxy as the only directing group ortho-Hydroxy carbonamides of the naphthalene series

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inks, Pencil-Leads, Or Crayons (AREA)

Abstract

The invention discloses a kind of permanent bordeaux pigment and preparation method thereof with strong dispersibility.This kind of pigment includes following component by weight: 10-25 parts of large red-based g, 20-30 parts of azoic coupling component AS, 1-3 parts of natrium dehydrocholicum, sub- 15-30 parts of sodium, 7-10 parts of liquid alkaline, 15-20 parts of hydrochloric acid, 3-6 parts of sodium acetate, 2-5 parts of sulfamic acid and 3-7 parts of auxiliary agent.By adding natrium dehydrocholicum to change the size of pigment particles, surface energy makes entire pigment have good mobility, prevents pigment flocculation this kind of pigment.

Description

A kind of permanent bordeaux pigment and preparation method thereof with strong dispersibility
Technical field
The present invention relates to technical field of chemical pigments, and in particular to a kind of permanent bordeaux pigment and its system with strong dispersibility Preparation Method.
Background technique
In aqueous ink most adding ingredient be permanent bordeaux 688, but in practical applications entire dispersion cannot with it is first Beginning dispersity is consistent, and flocculation phenomenon occurs, then forms biggish pigment aggregation speed in eddy motion and slows down, can make It separates at pigment, shoals sometimes, form piebald sometimes.
Summary of the invention
It is an object of the present invention in view of the above shortcomings of the prior art, propose a kind of permanent bordeaux with strong dispersibility Pigment and preparation method thereof, this kind of pigment make pigment possess good mobility in aqueous ink by addition deflocculant.
A kind of permanent bordeaux pigment with strong dispersibility proposed by the present invention includes following component: large red by weight G10-25 parts of base, 20-30 parts of azoic coupling component AS, 1-3 parts of natrium dehydrocholicum, sub- 15-30 parts of sodium, 7-10 parts of liquid alkaline, 15-20 parts of hydrochloric acid, 3-6 parts of sodium acetate, 2-5 parts of sulfamic acid and 3-7 parts of auxiliary agent.
It further, further include 110-150 parts and ice 60-80 parts of water.
Further, the auxiliary agent includes 2-3 parts and polysorbas20 1-4 parts of Magnesium succinate by mass parts.
Further, the carboxyl in negative point is introduced in the polysorbas20 molecule.
Further, the sub- sodium is one of sodium nitrite and sodium sulfite or two kinds
A kind of preparation method of the permanent bordeaux pigment with strong dispersibility, comprising the following steps:
(1), the preparation of diazo liquid: hydrochloric acid being added into water, opens stirring adjustment electric machine frequency 45Hz and large red-based g and dehydrogenation is added Sodium taurocholate, dissolution is complete, on the rocks, adjusts temperature -1~0 degree, and fast plus sub- sodium, survey KI test paper is more blue, stirs 40-50 minutes, KI examination Paper range is micro- blue-slightly blue, and sulfamic acid is added portionwise, stirs 5-15 minutes, micro- indigo plant-colourless, the temperature < 5 of KI test paper range Degree, obtains diazo liquid;
(2), the preparation of coupling solution: auxiliary agent being added into water, and stirring motor frequency is 40Hz, is warming up to 70-75 degree and azoic coupling component is added Liquid alkaline is added in AS, stirs dissolution in 20 minutes completely, and ice cooling is added immediately, obtains coupling liquid;
(3), it is coupled: opening stirring adjustment motor speed frequency 30Hz and sodium acetate is added, check and corrected acidometer, open circulation Pump adjusts motor speed frequency 50Hz, is stirred to coupling solution, adds diazo liquid after 2 minutes.Coupling solution is at 30-35 points It is added in clock, diazo liquid adds in 35-40 minutes, it is desirable that coupling solution first discharges.Coupling finishes 20 degree of temperature or so, the micro- mistake of diazonium Amount.Motor speed frequency 30Hz is adjusted, is stirred 1 hour, 70-75 degree is warming up to, keeps the temperature 30-35 minutes, cools down 60~65 degree, obtains To finished product.
Further, solution temperature is 55-65 DEG C in step (1).
Further, on the rocks in step (2) to be cooled to 16-18 DEG C.
Further, the coupled processes pH in step (3) is 6.0-8.0, and it is 6.5-7.5 that coupling, which terminates pH,.
Further, the couple temperature in is 18-20 DEG C.
A kind of permanent bordeaux pigment and preparation method thereof with strong dispersibility of the invention, this kind of pigment is by adding dehydrogenation gallbladder Sour sodium changes the size of pigment particles, and surface energy makes entire pigment have good mobility, prevents pigment flocculation.
Specific embodiment
For present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate this hair It is bright rather than limit the scope of the invention.In addition, various changes or modification that those skilled in the art make the present invention, this A little equivalent forms are equally fallen in the application range claimed.Proportion in the embodiment of the present invention is by weight.
Embodiment 1
Diazo liquid preparation:
In diazonium bucket plus water 5600L, hydrochloric acid is added, opens stirring adjustment electric machine frequency 45Hz and 10 parts of large red-based g is added and goes 1 part of hydrogen sodium taurocholate, 55 degree are warming up to, dissolution (checks 2-3 times) completely, and on the rocks, adjustment temperature -1 is spent, and fast plus sub- 15 parts of sodium is surveyed KI test paper is more blue, stirs 45 minutes, and KI test paper is micro- blue-slightly blue, and sulfamic acid is added portionwise, stirs 10 minutes, KI test paper is micro- Indigo plant-colourless, volume 13000L, 5 degree of temperature <.
Coupling solution preparation:
In dissolving bucket plus water discharges water 5500L, opens stirring, and adjustment electric machine frequency 40Hz is warming up to 70 degree of addition azoic coupling component AS 20 Part, 2 parts of Magnesium succinate and 1 part of polysorbas20 are added 7 parts of liquid alkaline, stir dissolution in 20 minutes completely, and 16 degree of ice adjustment is added immediately, Volume 13000L, 18 degree of temperature wait be coupled.
Coupling and heat preservation:
Discharge water about 2000 L in coupling bucket, opens sodium acetate 3-6 parts of addition of stirring adjustment motor speed frequency 30Hz, inspection and school Just acidometer opens circulating pump, adjusts temperature 18-20 degree, adjusts motor speed frequency 50Hz, is first comparatively fast put into coupling solution Into coupling bucket, diazo liquid is added after 2 minutes.Entire coupled processes control pH=6.0, and coupling solution adds in 30 minutes, Diazo liquid adds in 35 minutes, it is desirable that coupling solution first discharges.Coupling finishes 20 degree of temperature or so, the micro- excess of diazonium.Adjust motor Speed-frequency 30Hz is stirred 1 hour, pH=6.5, is warming up to 70 degree, keeps the temperature 30 minutes, is cooled down 60 degree, is obtained finished product.
Embodiment 2
Diazo liquid preparation:
In diazonium bucket plus water 5600L, hydrochloric acid is added, opens stirring adjustment electric machine frequency 45Hz and 17 parts of large red-based g is added and goes 2 parts of hydrogen sodium taurocholate, 60 degree are warming up to, dissolution (checks 2-3 times) completely, and on the rocks, adjustment temperature -1 is spent, and fast plus sub- 18 parts of sodium is surveyed KI test paper is more blue, stirs 45 minutes, and KI test paper is micro- blue-slightly blue, and sulfamic acid is added portionwise, stirs 10 minutes, KI test paper is micro- Indigo plant-colourless, volume 13000L, 5 degree of temperature <.
Coupling solution preparation:
In dissolving bucket plus water discharges water 5500L, opens stirring, and adjustment electric machine frequency 40Hz is warming up to 72 degree of addition azoic coupling component AS 25 Part, 3 parts of Magnesium succinate and 3 parts of polysorbas20 are added 8 parts of liquid alkaline, stir dissolution in 20 minutes completely, and 17 degree of ice adjustment is added immediately, Volume 13000L, 19 degree of temperature wait be coupled.
Coupling and heat preservation:
Discharge water about 2000 L in coupling bucket, opens stirring adjustment motor speed frequency 30Hz and is added 4 parts of sodium acetate, checks and correct Good acidometer opens circulating pump, adjusts 19 degree of temperature, adjusts motor speed frequency 50Hz, coupling solution is comparatively fast first put into idol It closes in bucket, adds diazo liquid after 2 minutes.Entire coupled processes control pH=7.0, and coupling solution adds in 32 minutes, diazonium Liquid adds in 38 minutes, it is desirable that coupling solution first discharges.Coupling finishes 20 degree of temperature or so, the micro- excess of diazonium.Adjust motor speed Frequency 30Hz is stirred 1 hour, pH=7.0, is warming up to 725 degree, keeps the temperature 32 minutes, is cooled down 62 degree, is obtained finished product.
Embodiment 3
Diazo liquid preparation:
In diazonium bucket plus water 5600L, hydrochloric acid is added, opens stirring adjustment electric machine frequency 45Hz and 25 parts of large red-based g is added and goes 3 parts of hydrogen sodium taurocholate, 65 degree are warming up to, dissolution (checks 2-3 times) completely, it is on the rocks, 0 degree of temperature is adjusted, fast plus sub- 30 parts of sodium surveys KI Test paper is more blue, stirs 45 minutes, and KI test paper is micro- blue-slightly blue, and sulfamic acid is added portionwise, stirs 10 minutes, the micro- indigo plant-of KI test paper It is colourless, 5 degree of volume 13000L, temperature <.
Coupling solution preparation:
In dissolving bucket plus water discharges water 5500L, opens stirring, adjustment electric machine frequency 40Hz, be warming up to 75 degree of AS30 parts of addition azoic coupling components, 3 parts and 4 parts of polysorbas20 of Magnesium succinate, 10 parts of liquid alkaline are added, stirs dissolution in 20 minutes completely, ice is added immediately and adjusts 18 degree, body Product 13000L, 20 degree of temperature wait be coupled.
Coupling and heat preservation:
Discharge water about 2000 L in coupling bucket, opens stirring adjustment motor speed frequency 30Hz and is added 6 parts of sodium acetate, checks and correct Good acidometer opens circulating pump, adjusts 20 degree of temperature, adjusts motor speed frequency 50Hz, coupling solution is comparatively fast first put into idol It closes in bucket, adds diazo liquid after 2 minutes.Entire coupled processes control pH=8.0, and coupling solution adds in 35 minutes, diazonium Liquid adds in 40 minutes, it is desirable that coupling solution first discharges.Coupling finishes 20 degree of temperature or so, the micro- excess of diazonium.Adjust motor speed Frequency 30Hz is stirred 1 hour, pH=7.5, is warming up to 75 degree, keeps the temperature 35 minutes, is cooled down 65 degree, is obtained finished product.
Exemplary illustration is carried out to the embodiment of the present invention above, but the content is only preferable implementation of the invention Example, should not be considered as limiting the scope of the invention.All the changes and improvements etc. of all application ranges according to the present invention, It should all fall within the scope of the patent of the present invention.

Claims (10)

1. a kind of permanent bordeaux pigment with strong dispersibility, which is characterized in that by weight include following component: erie Congo base G10-25 parts, 20-30 parts of azoic coupling component AS, 1-3 parts of natrium dehydrocholicum, sub- 15-30 parts of sodium, 7-10 parts of liquid alkaline, 15-20 parts of hydrochloric acid, vinegar Sour sodium 3-6 parts, 2-5 parts of sulfamic acid and 3-7 parts of auxiliary agent.
2. a kind of permanent bordeaux pigment with strong dispersibility as described in claim 1, it is characterised in that: further include water 110- 150 parts and ice 60-80 parts.
3. a kind of permanent bordeaux pigment with strong dispersibility as described in claim 1, it is characterised in that: the auxiliary agent presses quality Part includes Magnesium succinate 2-3 parts and polysorbas20 1-4 parts.
4. a kind of permanent bordeaux pigment with strong dispersibility as claimed in claim 3, it is characterised in that: the polysorbas20 molecule The middle carboxyl introduced in negative point.
5. a kind of permanent bordeaux pigment with strong dispersibility as described in claim 1, it is characterised in that: the Asia sodium is nitrous One of sour sodium and sodium sulfite or two kinds.
6. a kind of preparation method of permanent bordeaux pigment with strong dispersibility as described in claim 1-5 any one, special Sign is: the following steps are included:
(1), the preparation of diazo liquid: hydrochloric acid being added into water, opens stirring adjustment electric machine frequency 45Hz and large red-based g and dehydrogenation is added Sodium taurocholate, dissolution is complete, on the rocks, adjusts temperature -1~0 degree, and fast plus sub- sodium, survey KI test paper is more blue, stirs 40-50 minutes, KI examination Paper range is micro- blue-slightly blue, and sulfamic acid is added portionwise, stirs 5-15 minutes, micro- indigo plant-colourless, the temperature < 5 of KI test paper range Degree, obtains diazo liquid;
(2), the preparation of coupling solution: auxiliary agent being added into water, and stirring motor frequency is 40Hz, is warming up to 70-75 degree and azoic coupling component is added Liquid alkaline is added in AS, stirs dissolution in 20 minutes completely, and ice cooling is added immediately, obtains coupling liquid;
(3), it is coupled: opening stirring adjustment motor speed frequency 30Hz and sodium acetate is added, check and corrected acidometer, open circulation Pump adjusts motor speed frequency 50Hz, is stirred to coupling solution, diazo liquid is added after 2 minutes, coupling solution is at 30-35 points It is added in clock, diazo liquid adds in 35-40 minutes, it is desirable that coupling solution first discharges, and coupling finishes 20 degree of temperature or so, the micro- mistake of diazonium Amount adjusts motor speed frequency 30Hz, stirs 1 hour, is warming up to 70-75 degree, keeps the temperature 30-35 minutes, cools down 60~65 degree, obtains To finished product.
7. a kind of preparation method of the permanent bordeaux pigment with strong dispersibility as claimed in claim 6, it is characterised in that: step (1) solution temperature is 55-65 DEG C in.
8. a kind of preparation method of the permanent bordeaux pigment with strong dispersibility as claimed in claim 6, it is characterised in that: step (2) on the rocks in be cooled to 16-18 DEG C.
9. a kind of preparation method of the permanent bordeaux pigment with strong dispersibility as claimed in claim 6, it is characterised in that: step (3) the coupled processes pH in is 6.0-8.0, and it is 6.5-7.5 that coupling, which terminates pH,.
10. a kind of preparation method of the permanent bordeaux pigment with strong dispersibility as claimed in claim 6, it is characterised in that: step Suddenly the couple temperature in (3) is 18-20 DEG C.
CN201811397605.3A 2018-11-22 2018-11-22 A kind of permanent bordeaux pigment and preparation method thereof with strong dispersibility Pending CN109385116A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102746708A (en) * 2012-05-28 2012-10-24 吴江市屯村颜料厂 Preparation method of permanent red S2BL
CN103265821A (en) * 2013-05-22 2013-08-28 南通市争妍颜料化工有限公司 High-covering power one-step production process of permanent bordeaux F5RK
CN105907127A (en) * 2016-05-26 2016-08-31 济宁阳光化学有限公司 Method for producing environment-friendly organic pigment permanent bordeaux FGR
CN106243771A (en) * 2016-07-29 2016-12-21 山东阳光颜料有限公司 A kind of preparation method of bonding agent printing aqueous color paste paratonere 22
CN107163614A (en) * 2017-06-06 2017-09-15 宣城英特颜料有限公司 A kind of permanent bordeaux pigment and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102746708A (en) * 2012-05-28 2012-10-24 吴江市屯村颜料厂 Preparation method of permanent red S2BL
CN103265821A (en) * 2013-05-22 2013-08-28 南通市争妍颜料化工有限公司 High-covering power one-step production process of permanent bordeaux F5RK
CN105907127A (en) * 2016-05-26 2016-08-31 济宁阳光化学有限公司 Method for producing environment-friendly organic pigment permanent bordeaux FGR
CN106243771A (en) * 2016-07-29 2016-12-21 山东阳光颜料有限公司 A kind of preparation method of bonding agent printing aqueous color paste paratonere 22
CN107163614A (en) * 2017-06-06 2017-09-15 宣城英特颜料有限公司 A kind of permanent bordeaux pigment and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
侯惠民 等编著: "《药用辅料应用技术(第二版)》", 31 July 2002, 中国医药科技出版社 *

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Application publication date: 20190226