CN103923480A - Preparation method of orange benzimidazolone azo pigment - Google Patents
Preparation method of orange benzimidazolone azo pigment Download PDFInfo
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- CN103923480A CN103923480A CN201410159244.4A CN201410159244A CN103923480A CN 103923480 A CN103923480 A CN 103923480A CN 201410159244 A CN201410159244 A CN 201410159244A CN 103923480 A CN103923480 A CN 103923480A
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Abstract
The invention discloses a preparation method of an orange benzimidazolone azo pigment. The preparation method comprises the following steps: diazotization, precipitation, coupling, pigmentation, filter pressing for the first time, pulping, postprocessing, filter pressing for the second time and drying. The preparation method has the beneficial effects that the product has good stability and stable various performance indexes, the yield of products can be improved, the discharge is reduced, the treatment cost of waste gas, waste water, and solid waste is reduced, and social benefit and economic benefit are excellent. The obtained product has gorgeous colored light, high tinting strength, good dispersibility and fluidity, can be used for production of exterior wall coating materials, finishing varnish and refinishing paint of saloon cars, top-grade plastic products, top-grade printing ink products and the like.
Description
Technical field
The present invention relates to a kind of preparation method of orange benzoglyoxaline ketone azo pigment.
Background technology
The problems such as value that current domestic pigment dyestuff enterprise exists that material consumption energy consumption is high, yield is low, relies on end treatment, ton product is created is low.Compare with area with developed country, face larger environmental protection pressure.Aspect product innovation capability, production technology level, Environmental Protection Level especially environmental protection innovative technology and innovative product, also there is very large gap with international most advanced level, the technical progress of pigment dyestuff industry should be served as theme and carries out along being improved environmental benefit.
Therefore, be badly in need of a kind of improved technology and solve existing this problem in prior art.
Summary of the invention
The invention provides a kind of preparation method of orange benzoglyoxaline ketone azo pigment of the yield that improves product.
The technical solution used in the present invention is:
A preparation method for orange benzoglyoxaline ketone azo pigment, comprises the following steps:
Diazonium: add red base 3GL, hydrochloric acid, Glacial acetic acid and water making beating in doazo reaction still, the frozen water that adds again 500-700 part stirs 30-240 minute, then sodium nitrite solution is slowly joined in reactor, carry out diazotization reaction, reaction stirring adds thionamic acid and destroys after 60-240 minute, add the processing of decolouring of carclazyte gac, then filter, filtrate is for subsequent use; In another reactor, add AABI and liquid caustic soda, to stir and carry out suction filtration after 30-240 minute, filtrate is for subsequent use;
Separate out: the AABI having dissolved puts into coupled reaction still, add the Glacial acetic acid of 200-400 part, it is separated out, the PH having separated out is 4-7, then add 400-500 part sodium-acetate, stablizing its PH is 5-7;
Coupling: the diazo liquid having reacted is added in the coupling component of having separated out;
Pigmenting: it is heat-treated, make it be warming up to 80-85 DEG C, soaking time is 4-5 hour;
Press filtration for the first time: the water that the adds 400-600 part filtration of lowering the temperature, rinsing obtains filter cake;
Making beating: add the water making beating of 1500-2000 part, pulled an oar and added the auxiliary agent 20 of 20-50 part, the liquid caustic soda of 150-300 part, does alkaline purification, is warming up to 80-90 DEG C, insulation 2-3 hour, after add water for cooling, filter, rinsing, obtains filter cake;
Aftertreatment: filter cake making beating adds the water of 1000-1200 part, and the auxiliary agent 10 that adds 200-300 part, is warming up to 140-145 DEG C, 0.4-0.5MPA, insulation 2-3 hour;
Press filtration for the second time: be cooled to 35-45 DEG C of filtration with chuck, rinsing, obtains filter cake;
Dry: filter cake enters baking oven 60-70 DEG C oven dry, is pigment orange ZHL-70.
Red base 3GL in described diazonium step: hydrochloric acid: Glacial acetic acid: Sodium Nitrite: the mass ratio of water is 200:(400-800): (1000-2000): (200-250): (200-400), AABI: the mass ratio of liquid caustic soda is (200-220): (300-600).
In described diazonium step, diazotization reaction temperature is-5-5 DEG C.
In described diazonium step, detect with starch potassium iodide paper when diazotization reaction, keep test paper color to be blue.
In described coupling step, the complete diazo component of coupling is inexcessive, detects with detecting liquid.
In described press filtration step, color is changed into orange redly by black or brown, and filter cake rinsing is to neutral.
The pigment orange ZHL-70 technological process of production is:
Separate out-> of diazonium-> coupling-> pigmenting-> is press filtration-> making beating-> aftertreatment-> press filtration-> oven dry-> pulverizing-> inspection-> packaging for the second time for the first time.
The chemical formula of doazo reaction is:
The chemical formula of coupled reaction is:
The invention has the beneficial effects as follows: product stability is good, property indices is stable, can improve the yield of product, reduce discharge, reduce three wastes processing cost, have and reached good Social benefit and economic benefit, its coloured light of products obtained therefrom is gorgeous, tinting strength is high, easily disperse good and good fluidity, can be used for the production of finishing paint and retouching paint, high-grade plastics and the high-grade ink goods etc. of exterior coating, car.
Embodiment
Embodiment 1
The preparation method of a kind of orange benzoglyoxaline ketone azo pigment of the present invention, comprises the following steps:
Diazonium: add hydrochloric acid, the Glacial acetic acid of 1000kg and the making beating of the water of 200kg of 3GL, the 400kg of red base 200kg in doazo reaction still, the frozen water that adds again 600kg stirs 30 minutes, then the sodium nitrite solution of 200kg is slowly joined in reactor, carry out diazotization reaction, temperature is controlled at-5 DEG C, detect with starch potassium iodide paper, keep test paper color to be blue, reaction is stirred and after 60 minutes, is added thionamic acid and destroy, and adds the processing of decolouring of carclazyte gac, then filter, filtrate is for subsequent use; In another reactor, add the AABI of 200kg and the liquid caustic soda of 300kg, to stir and carry out suction filtration after 30 minutes, filtrate is for subsequent use;
Separate out: the AABI having dissolved puts into coupled reaction still, add the Glacial acetic acid of 200kg, it is separated out, the PH having separated out is 47, then add 400kg sodium-acetate, stablizing its PH is 5.5;
Coupling: the diazo liquid having reacted is added in the coupling component of having separated out, the complete diazo component of coupling is inexcessive, detects with detecting liquid;
Pigmenting: it is heat-treated, make it be warming up to 80 DEG C, soaking time is 4 hours;
Press filtration for the first time: the water that the adds 400kg filtration of lowering the temperature, rinsing obtains filter cake, and color is changed into orange red by black or brown, and filter cake rinsing is to neutral;
Making beating: add the water making beating of 1500kg, pulled an oar and added the auxiliary agent 20 of 20kg, the liquid caustic soda of 200kg, does alkaline purification, is warming up to 80 DEG C, be incubated 2 hours, after add water for cooling, filtration, rinsing, obtains filter cake;
Aftertreatment: filter cake making beating adds the water of 1000kg, adds the auxiliary agent 10 of 200kg, is warming up to 140 DEG C, and 0.45MPA, is incubated 3 hours;
Press filtration for the second time: be cooled to 35 DEG C of filtrations with chuck, rinsing, obtains filter cake;
Dry: filter cake enters 70 DEG C of oven dry of baking oven, is pigment orange ZHL-70.
Embodiment 2
The preparation method of a kind of orange benzoglyoxaline ketone azo pigment of the present invention, comprises the following steps:
Diazonium: add hydrochloric acid, the Glacial acetic acid of 1250kg and the making beating of the water of 300kg of 3GL, the 500kg of red base 200kg in doazo reaction still, the frozen water that adds again 600kg stirs 30-240 minute, then the sodium nitrite solution of 220kg is slowly joined in reactor, carry out diazotization reaction, temperature is controlled at 0 DEG C, detect with starch potassium iodide paper, keep test paper color to be blue, reaction stirring adds thionamic acid and destroys after 120 minutes, add the processing of decolouring of carclazyte gac, then filter, filtrate is for subsequent use; In another reactor, add the AABI of 310kg and the liquid caustic soda of 400kg, to stir and carry out suction filtration after 45 minutes, filtrate is for subsequent use;
Separate out: the AABI having dissolved puts into coupled reaction still, add the Glacial acetic acid of 250kg, it is separated out, the PH having separated out is 6, then add 500kg sodium-acetate, stablizing its PH is 6.5;
Coupling: the diazo liquid having reacted is added in the coupling component of having separated out, the complete diazo component of coupling is inexcessive, detects with detecting liquid;
Pigmenting: it is heat-treated, make it be warming up to 85 DEG C, soaking time is 4 hours;
Press filtration for the first time: the water that the adds 450kg filtration of lowering the temperature, rinsing obtains filter cake, and color is changed into orange red by black or brown, and filter cake rinsing is to neutral;
Making beating: add the water making beating of 1800kg, pulled an oar and added the auxiliary agent 20 of 50kg, the liquid caustic soda of 250kg, does alkaline purification, is warming up to 90 DEG C, be incubated 3 hours, after add water for cooling, filtration, rinsing, obtains filter cake;
Aftertreatment: filter cake making beating adds the water of 1100kg, adds the auxiliary agent 10 of 300kg, is warming up to 145 DEG C, and 0.5MPA, is incubated 2 hours;
Press filtration for the second time: be cooled to 40 DEG C of filtrations with chuck, rinsing, obtains filter cake;
Dry: filter cake enters 70 DEG C of oven dry of baking oven, is pigment orange ZHL-70.
Embodiment 3
The preparation method of a kind of orange benzoglyoxaline ketone azo pigment of the present invention, comprises the following steps:
Diazonium: add hydrochloric acid, the Glacial acetic acid of 1600kg and the making beating of the water of 300kg of 3GL, the 600kg of red base 200kg in doazo reaction still, the frozen water that adds again 550kg stirs 120 minutes, then the sodium nitrite solution of 230kg is slowly joined in reactor, carry out diazotization reaction, temperature is controlled at 3 DEG C, detect with starch potassium iodide paper, keep test paper color to be blue, reaction is stirred and after 120 minutes, is added thionamic acid and destroy, and adds the processing of decolouring of carclazyte gac, then filter, filtrate is for subsequent use; In another reactor, add the AABI of 210kg and the liquid caustic soda of 400kg, to stir and carry out suction filtration after 100 minutes, filtrate is for subsequent use;
Separate out: the AABI having dissolved puts into coupled reaction still, add the Glacial acetic acid of 280kg, it is separated out, the PH having separated out is 5, then add 440kg sodium-acetate, stablizing its PH is 6.5;
Coupling: the diazo liquid having reacted is added in the coupling component of having separated out, the complete diazo component of coupling is inexcessive, detects with detecting liquid;
Pigmenting: it is heat-treated, make it be warming up to 82 DEG C, soaking time is 4.5 hours;
Press filtration for the first time: the water that the adds 550kg filtration of lowering the temperature, rinsing obtains filter cake, and color is changed into orange red by black or brown, and filter cake rinsing is to neutral;
Making beating: add the water making beating of 1800kg, pulled an oar and added the auxiliary agent 20 of 30kg, the liquid caustic soda of 2500kg, does alkaline purification, is warming up to 88 DEG C, be incubated 2.5 hours, after add water for cooling, filtration, rinsing, obtains filter cake;
Aftertreatment: filter cake making beating adds the water of 1150kg, adds the auxiliary agent 10 of 280kg, is warming up to 143 DEG C, and 0.44MPA, is incubated 2.5 hours;
Press filtration for the second time: be cooled to 42 DEG C of filtrations with chuck, rinsing, obtains filter cake;
Dry: filter cake enters 68 DEG C of oven dry of baking oven, is pigment orange ZHL-70.
Embodiment 4
The preparation method of a kind of orange benzoglyoxaline ketone azo pigment of the present invention, comprises the following steps:
Diazonium: add hydrochloric acid, the Glacial acetic acid of 2000kg and the making beating of the water of 400kg of 3GL, the 800kg of red base 200kg in doazo reaction still, the frozen water that adds again 700kg stirs 240 minutes, then the sodium nitrite solution of 250kg is slowly joined in reactor, carry out diazotization reaction, temperature is controlled at 5 DEG C, detect with starch potassium iodide paper, keep test paper color to be blue, reaction is stirred and after 240 minutes, is added thionamic acid and destroy, and adds the processing of decolouring of carclazyte gac, then filter, filtrate is for subsequent use; In another reactor, add the AABI of 220kg and the liquid caustic soda of 00kg, to stir and carry out suction filtration after 240 minutes, filtrate is for subsequent use;
Separate out: the AABI having dissolved puts into coupled reaction still, add the Glacial acetic acid of 400kg, it is separated out, the PH having separated out is 6, then add 500kg sodium-acetate, stablizing its PH is 7;
Coupling: the diazo liquid having reacted is added in the coupling component of having separated out, the complete diazo component of coupling is inexcessive, detects with detecting liquid;
Pigmenting: it is heat-treated, make it be warming up to 85 DEG C, soaking time is 5 hours;
Press filtration for the first time: the water that the adds 600kg filtration of lowering the temperature, rinsing obtains filter cake, and color is changed into orange red by black or brown, and filter cake rinsing is to neutral;
Making beating: add the water making beating of 2000kg, pulled an oar and added the auxiliary agent 20 of 50kg, the liquid caustic soda of 300kg, does alkaline purification, is warming up to 90 DEG C, be incubated 3 hours, after add water for cooling, filtration, rinsing, obtains filter cake;
Aftertreatment: filter cake making beating adds the water of 1200kg, adds the auxiliary agent 10 of 300kg, is warming up to 145 DEG C, and 0.5MPA, is incubated 3 hours;
Press filtration for the second time: be cooled to 45 DEG C of filtrations with chuck, rinsing, obtains filter cake;
Dry: filter cake enters 70 DEG C of oven dry of baking oven, is pigment orange ZHL-70.
Product stability is good, property indices is stable, can improve the yield of product, reduce discharge, reduce three wastes processing cost, have and reached good Social benefit and economic benefit, its coloured light of products obtained therefrom is gorgeous, tinting strength is high, easily disperse good and good fluidity, can be used for the production of finishing paint and retouching paint, high-grade plastics and the high-grade ink goods etc. of exterior coating, car.
Claims (6)
1. a preparation method for orange benzoglyoxaline ketone azo pigment, is characterized in that: comprise the following steps:
Diazonium: add red base 3GL, hydrochloric acid, Glacial acetic acid and water making beating in doazo reaction still, the frozen water that adds again 500-700 part stirs 30-240 minute, then sodium nitrite solution is slowly joined in reactor, carry out diazotization reaction, reaction stirring adds thionamic acid and destroys after 60-240 minute, add the processing of decolouring of carclazyte gac, then filter, filtrate is for subsequent use; In another reactor, add AABI and liquid caustic soda, to stir and carry out suction filtration after 30-240 minute, filtrate is for subsequent use;
Separate out: the AABI having dissolved puts into coupled reaction still, add the Glacial acetic acid of 200-400 part, it is separated out, the PH having separated out is 4-7, then add 400-500 part sodium-acetate, stablizing its PH is 5-7;
Coupling: the diazo liquid having reacted is added in the coupling component of having separated out;
Pigmenting: it is heat-treated, make it be warming up to 80-85 DEG C, soaking time is 4-5 hour;
Press filtration for the first time: the water that the adds 400-600 part filtration of lowering the temperature, rinsing obtains filter cake;
Making beating: add the water making beating of 1500-2000 part, pulled an oar and added the auxiliary agent 20 of 20-50 part, the liquid caustic soda of 150-300 part, does alkaline purification, is warming up to 80-90 DEG C, insulation 2-3 hour, after add water for cooling, filter, rinsing, obtains filter cake;
Aftertreatment: filter cake making beating adds the water of 1000-1200 part, and the auxiliary agent 10 that adds 200-300 part, is warming up to 140-145 DEG C, 0.4-0.5MPA, insulation 2-3 hour;
Press filtration for the second time: be cooled to 35-45 DEG C of filtration with chuck, rinsing, obtains filter cake;
Dry: filter cake enters baking oven 60-70 DEG C oven dry, is pigment orange ZHL-70.
2. the preparation method of a kind of orange benzoglyoxaline ketone azo pigment according to claim 1, it is characterized in that: red base 3GL in described diazonium step: hydrochloric acid: Glacial acetic acid: Sodium Nitrite: the mass ratio of water is 200:(400-800): (1000-2000): (200-250): (200-400), AABI: the mass ratio of liquid caustic soda is (200-220): (300-600).
3. the preparation method of a kind of orange benzoglyoxaline ketone azo pigment according to claim 1, is characterized in that: in described diazonium step, diazotization reaction temperature is-5-5 DEG C.
4. the preparation method of a kind of orange benzoglyoxaline ketone azo pigment according to claim 1, is characterized in that: in described diazonium step, detect when diazotization reaction with starch potassium iodide paper, keep test paper color to be blue.
5. the preparation method of a kind of orange benzoglyoxaline ketone azo pigment according to claim 1, is characterized in that: in described coupling step, the complete diazo component of coupling is inexcessive, detects with detecting liquid.
6. the preparation method of a kind of orange benzoglyoxaline ketone azo pigment according to claim 1, is characterized in that: in described press filtration step for the first time, color is changed into orange redly by black or brown, and filter cake rinsing is to neutral.
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| CN201410159244.4A CN103923480A (en) | 2014-04-21 | 2014-04-21 | Preparation method of orange benzimidazolone azo pigment |
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| CN201410159244.4A CN103923480A (en) | 2014-04-21 | 2014-04-21 | Preparation method of orange benzimidazolone azo pigment |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104513494A (en) * | 2014-12-25 | 2015-04-15 | 上虞舜联化工有限公司 | Preparation method for pigment orange 64 with high color intensity |
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| US4195020A (en) * | 1973-09-21 | 1980-03-25 | Hoechst Aktiengesellschaft | Dichloro-phenyl-azo-acetoacetylamino-benzimidazolone pigments |
| JP2003026951A (en) * | 2001-07-12 | 2003-01-29 | Dainippon Ink & Chem Inc | Acetanilidobenzimidazolone azo pigment and method for producing the same |
| CN1563202A (en) * | 2004-04-16 | 2005-01-12 | 华东理工大学 | Method for preparing organic pigment of red benzimidazolones |
| CN1569968A (en) * | 2004-04-29 | 2005-01-26 | 华东理工大学 | Yellow, orange benzimidazolone like azo dye making method |
| CN102391664A (en) * | 2011-06-21 | 2012-03-28 | 南通市争妍颜料化工有限公司 | Preparation method of pigment orange 64 |
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2014
- 2014-04-21 CN CN201410159244.4A patent/CN103923480A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4195020A (en) * | 1973-09-21 | 1980-03-25 | Hoechst Aktiengesellschaft | Dichloro-phenyl-azo-acetoacetylamino-benzimidazolone pigments |
| JP2003026951A (en) * | 2001-07-12 | 2003-01-29 | Dainippon Ink & Chem Inc | Acetanilidobenzimidazolone azo pigment and method for producing the same |
| CN1563202A (en) * | 2004-04-16 | 2005-01-12 | 华东理工大学 | Method for preparing organic pigment of red benzimidazolones |
| CN1569968A (en) * | 2004-04-29 | 2005-01-26 | 华东理工大学 | Yellow, orange benzimidazolone like azo dye making method |
| CN102391664A (en) * | 2011-06-21 | 2012-03-28 | 南通市争妍颜料化工有限公司 | Preparation method of pigment orange 64 |
Non-Patent Citations (2)
| Title |
|---|
| 周春隆: "有机颜料粒径调整技术进展", 《精细与专用化学品》, vol. 15, no. 13, 6 July 2007 (2007-07-06) * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104513494A (en) * | 2014-12-25 | 2015-04-15 | 上虞舜联化工有限公司 | Preparation method for pigment orange 64 with high color intensity |
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Application publication date: 20140716 |