CN104479406B - A kind of solvent inkjet ink industrialized preparing process of transparent type high glaze pigment red 146 - Google Patents
A kind of solvent inkjet ink industrialized preparing process of transparent type high glaze pigment red 146 Download PDFInfo
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- CN104479406B CN104479406B CN201410750367.5A CN201410750367A CN104479406B CN 104479406 B CN104479406 B CN 104479406B CN 201410750367 A CN201410750367 A CN 201410750367A CN 104479406 B CN104479406 B CN 104479406B
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Abstract
A kind of solvent inkjet ink industrialized preparing process of transparent type high glaze pigment red 146, belongs to technical field of fine chemical synthesis.Comprise the steps：3 amino, 4 methoxybenzoyl aniline, water and hydrochloric acid are added in common response kettle, it is warming up to 30 DEG C, quick stirring 30 minutes, obtain dispersion liquid, sodium nitrite in aqueous solution is added in the dispersion liquid, carry out adding sodium acetate, emulsifying agent to obtain diazo solution after diazo-reaction is stirred 60 minutes, adding azoic coupling component AS LC stirring and obtaining flocculoreaction liquid carries out coupling reaction, then post-treated and heat up and turn brilliant reaction and obtain solvent inkjet ink transparent type high glaze pigment red 146.Reaction condition of the present invention is gentle, and low for equipment requirements, the reaction time is short, and emulsifying agent more typically and applies difficulty less, meets the novel environment friendly theme of promotion, the product bright in color light for obtaining, and its heat resistance reaches 220 DEG C/5min, fast light 5 grades.
Description
Technical field
The invention belongs to technical field of fine chemical synthesis, and in particular to a kind of compared with conventional blu-ray red solvent resistance
Good, the coloured light vivid solvent inkjet ink industrialized preparing process of transparent type high glaze pigment red 146.
Background technology
Pigment ratio C.I. pigment red 48:2、48:3 show blue light, than paratonere 57:1 slightly carries gold-tinted, and its advantageous feature is resistance to
Solvent, light resistance are good, and heat-resistant stability compares 57:1 is high 20 DEG C, and coloured light is vivid.It is mainly used in ink and coating, emulsion paint and building
Coating；Brown can be risked with pigment yellow 83, carbon black, for stain for wood.
In solvent inkjet ink direction, pigment red 146 belongs to medium-to-high grade organic pigment, it is desirable to good solvent resistance, bloom
Pool, good fluidity and higher transparency.Conventional pigment red 146 can not accomplish high gloss and the high grade of transparency, high transparency simultaneously
Degree and the product of good fluidity.One of production difficult point is the problems of dissolution of azoic coupling component intermediate A S-LC, and AS-LC solute effect is not
Directly result in well that coupling reaction is undesirable, and then the performance of product is affected, coloured light dark, gloss difference partially.
The two of difficult point are that post processing heats up and turn brilliant colourshifting process that the high crystal formation of temperature obtains then poor transparency of growing up；Temperature
Low, do not change colour or change colour not exclusively then coloured light obfuscation, mobility, gloss difference.
Content of the invention
For the above-mentioned problems in the prior art, it is an object of the invention to provide a kind of solvent inkjet ink is high with transparent type
The industrialized preparing process of colour lustre pigments red 146, solves apthol AS-LC through optimize technique, adjustment formula and dissolves difficult point, heat up
Annesl process so that reaction fully completely, obtains the product of excellent performance.
A kind of described solvent inkjet ink industrialized preparing process of transparent type high glaze pigment red 146, it is characterised in that bag
Include following steps：
1）Acid out salt-forming reaction：3- amino-4-methoxyl benzanilide, water and hydrochloric acid are added in common response kettle,
30 DEG C are warming up to, quick stirring 30 minutes, obtain dispersion liquid；
2）Diazo-reaction：Under acid condition, to step 1 at a temperature of -10 DEG C～10 DEG C）In the dispersion liquid for obtaining, 2-5
Sodium nitrite in aqueous solution is added in minute, carry out adding sodium acetate, emulsifying agent to obtain diazonium after diazo-reaction is stirred 60 minutes
Change solution；
3）Water, liquid caustic soda, chaotropic agent are added in dissolving reactor, 85-90 DEG C under stirring, is warming up to, add apthol AS-LC
Stirring obtains flocculoreaction liquid；
4）Coupling reaction：Controlling reaction temperature at 0 DEG C～15 DEG C, by step 3）In the settled solution 30-60 minute for obtaining
Add step 2）Coupling reaction kettle in carry out coupling reaction, it is 5.5-6 to control reaction pH with 5% hydrochloric acid in course of reaction, and protects
Temperature stirring terminates for 1 ~ 2 hour to reaction；
5）Post processing：To step 4）Coupling reaction kettle in the clear rosin liquid of additionization, plus rosin liquid time control is in 1-
In 10 minutes；
6）Heat up and turn brilliant reaction：By step 5）Reactant liquor, be warming up to 70 ~ 100 DEG C, insulation reaction 30 minutes, then be down to
Room temperature, filters, and dries and obtain solvent inkjet ink transparent type high glaze pigment red 146 at 80 ~ 110 DEG C.
A kind of described solvent inkjet ink industrialized preparing process of transparent type high glaze pigment red 146, it is characterised in that step
Rapid 2）Described in 3- amino-4-methoxyl benzanilide and emulsifying agent mass ratio be 1：0.01 ~ 0.06, emulsifying agent is MOA-4.
A kind of described solvent inkjet ink industrialized preparing process of transparent type high glaze pigment red 146, it is characterised in that step
Rapid 3）Described apthol AS-LC is 1 with the mass ratio of chaotropic agent：0.02~0.1.
A kind of described solvent inkjet ink industrialized preparing process of transparent type high glaze pigment red 146, it is characterised in that step
Rapid 3）Described chaotropic agent is alcohol, the one kind in MOA-4, OS-15 or detergent 209, MOA-4, OS-15 of the present invention and washes
Wash agent 209 and be commercially available prod.
A kind of described solvent inkjet ink industrialized preparing process of transparent type high glaze pigment red 146, it is characterised in that step
Rapid 3）Described liquid caustic soda：Apthol AS-LC mol ratio is 1-3：1.
A kind of described solvent inkjet ink industrialized preparing process of transparent type high glaze pigment red 146, it is characterised in that step
Rapid 3）Described apthol AS-LC：Liquid caustic soda mol ratio is 1：2-3.
A kind of described solvent inkjet ink industrialized preparing process of transparent type high glaze pigment red 146, it is characterised in that step
Rapid 5）It is 70～100 DEG C that described post processing heats up.
A kind of described solvent inkjet ink industrialized preparing process of transparent type high glaze pigment red 146, it is characterised in that step
Rapid 5）Described apthol AS-LC：The mass ratio of rosin is 1：0.02～0.1.
The paratonere of present invention synthesis, its reaction equation are as follows：
By adopting above-mentioned technology, compared with prior art, beneficial effects of the present invention are as follows：
1）The present invention is by adjusting 2- hydroxyl -3- naphthoyl-(the chloro- 2,5- bi-methoxy of 4-) aniline with liquid caustic soda proportioning extremely
1：2-3, and add chaotropic agent, preferably detergent 209 so that apthol AS-LC solute effect is maximized；
2）The present invention adopts obforms coupling process, adds sodium acetate and ensure that reaction system is in solutions of weak acidity in diazo component
Under so that reaction is abundant, stable；Again by controlling emulsification dosage, control and turn brilliant effect, the product cut size distribution for so obtaining
Concentrate, bright, good fluidity, high transparency, and the clear rosin liquid of present invention additionization in post processing, improve further
Its transparency and glossiness；
3）Reaction condition of the present invention is gentle, and low for equipment requirements, the reaction time is short, and emulsifying agent more typically and applies difficulty relatively
Little, meet the novel environment friendly theme of promotion, the product bright in color light for obtaining, its heat resistance reach 220 DEG C/5min, fast light 5 grades.
Description of the drawings
Fig. 1 is apthol AS-LC mol ratio and the precipitation capacity graph of relation of the present invention；
Fig. 2 is solute effect figure of the different detergent of the present invention to apthol AS-LC.
Specific embodiment
With reference to specific embodiment, the present invention will be further described, but embodiment does not limit the protection model of the present invention
Enclose.
Embodiment 1：Apthol AS-LC solubility parameter determines
1）Common response kettle adds water 150ml, 30% liquid caustic soda 8.2g～20g, opens stirring, is heated to 85-90 DEG C, plus
Enter AS-LC 186kg clear to stirring and dissolvingization, sediment is filtered to obtain, dry and weight of precipitate is weighed, how much sentenced by sediment
Disconnected solute effect.As following table：
Can be seen that from upper table and Fig. 1 and work as liquid caustic soda：AS-LC mol ratio ＞ 1.4, sediment amount tend towards stability value >=1.0g.
2）Choose liquid caustic soda：Apthol AS-LC mol ratio is 2.5, compares alcohol, MOA-4, OS-15 rush different from detergent 209
The effect of solvent, as a result as shown in Fig. 2 from figure 2 it can be seen that alcohol and solute effect of the detergent 209 to apthol AS-LC
Most preferably, because alcohol is relatively hazardous, be not suitable for industrialized production, so detergent 209 is chosen as chaotropic agent.
Embodiment 2：The synthesis modification research of pigment red 146
1）Common response kettle adds 150ml water, the hydrochloric acid of 20g content 30%, addition 12g 3- amino-4-methoxyl benzoyl
Aniline stirs 30min；Then it is little diazotising stirring reaction 1 to be carried out in 0 DEG C of sodium nitrite solution 11.5g for being slowly added to 30%
When, excessive nitrite sodium sulfamic acid is removed and obtains diazo liquid；- 4 0.2g is direct for industrial sodium acetate 40g, Emulsifier MOA
Diazo liquid reaction stirring 10 minutes is added, i.e. diazo liquid is prepared and completed；Coupling reaction kettle is placed into, regulating pondage 100ml treats idol
Close reaction.
2）Common response kettle adds water 150g, 30% liquid caustic soda 17.1g, detergent 209,0.92g, opens stirring, is warming up to 85-
90 DEG C, add apthol AS-LC 18.6g clear to stirring and dissolvingization；Then quickly on the rocks be cooled to 20-25 DEG C, adjustment liquid measure treat instead
Should.
3）Anti- coupling reaction is carried out in the coupling reaction kettle by adding at 0-15 DEG C of coupling component liquid, maintain the reaction time
50-60min, controls terminal pH=5.5-6, and diazo liquid is stirred 1.5 hours after adding；
4）Post-processing stages are warmed up to 90-95 DEG C, are incubated 30 minutes, suction filtration of lowering the temperature, and obtain paratonere in 85 DEG C of drying
30g, the application performance of the paratonere：Fast light 5 grades, heat-resisting 220 DEG C；Transparency △ L*=1.20（Judgement -0.5T）, glossiness：
Embodiment 3：The synthesis modification research of pigment red 146
1）Common response kettle adds 150ml water, the hydrochloric acid of 20g content 30%, addition 12g 3- amino-4-methoxyl benzoyl
Aniline stirs 30min；Then it is little diazotising stirring reaction 1 to be carried out in 0 DEG C of sodium nitrite solution 11.5g for being slowly added to 30%
When, excessive nitrite sodium sulfamic acid is removed and obtains diazo liquid；- 4 0.2g is direct for industrial sodium acetate 40g, Emulsifier MOA
Diazo liquid reaction stirring 10 minutes is added, i.e. diazo liquid is prepared and completed；Coupling reaction kettle is placed into, regulating pondage 100ml treats idol
Close reaction.
2）Common response kettle adds water 150g, 30% liquid caustic soda 17.1g, detergent 209,1.2g, opens stirring, is warming up to 85-90
DEG C, add apthol AS-LC 18.6g clear to stirring and dissolvingization；Then quickly on the rocks be cooled to 20-25 DEG C, adjustment liquid measure treat instead
Should.
3）Anti- coupling reaction is carried out in the coupling reaction kettle by adding at 0-15 DEG C of coupling component liquid, maintain the reaction time
30-40min, controls terminal pH=5.5-6, and diazo liquid is stirred 1 hour after adding；
4）Post-processing stages, rapidly join in coupling reaction kettle after 3g rosin intensificationization is clear, heat up after stirring 10min
To 85-90 DEG C, 30 minutes are incubated, suction filtration of lowering the temperature, pigment red 3 3g, the application performance of the paratonere is obtained in 85 DEG C of drying：Fast light
4 grades, heat-resisting 200 DEG C；Transparency △ L*=-2.32（Judge 1.5T）, glossiness：
Embodiment 4：The synthesis modification research of pigment red 146
1）Common response kettle adds 150ml water, the hydrochloric acid of 20g content 30%, addition 12g 3- amino-4-methoxyl benzoyl
Aniline stirs 30min；Then it is little diazotising stirring reaction 1 to be carried out in 0 DEG C of sodium nitrite solution 11.5g for being slowly added to 30%
When, excessive nitrite sodium sulfamic acid is removed and obtains diazo liquid；- 4 0.2g is direct for industrial sodium acetate 40g, Emulsifier MOA
Diazo liquid reaction stirring 10 minutes is added, i.e. diazo liquid is prepared and completed；Coupling reaction kettle is placed into, regulating pondage 100ml treats idol
Close reaction.
2）Common response kettle adds water 150g, 30% liquid caustic soda 17.1g, detergent 209,0.72g, opens stirring, is warming up to 85-
90 DEG C, add apthol AS-LC 18.6g clear to stirring and dissolvingization；Then quickly on the rocks be cooled to 20-25 DEG C, adjustment liquid measure treat instead
Should.
3）Anti- coupling reaction is carried out in the coupling reaction kettle by adding at 0-15 DEG C of coupling component liquid, maintain the reaction time
40-50min, controls terminal pH=5.5-6, and diazo liquid is stirred 1 hour after adding；
4）Post-processing stages, rapidly join in coupling reaction kettle after 1g rosin intensificationization is clear, heat up after stirring 10min
To 90-95 DEG C, 30 minutes are incubated, suction filtration of lowering the temperature, pigment red 3 1g, the application performance of the paratonere is obtained in 85 DEG C of drying：The face
The red application performance of material：Fast light 5 grades, heat-resisting 210 DEG C；Transparency △ L*=-0.86（Judge 0.5T）, glossiness：
Claims (5)
1. a kind of solvent inkjet ink industrialized preparing process of transparent type high glaze pigment red 146, it is characterised in that including following step
Suddenly：
1）Acid out salt-forming reaction：3- amino-4-methoxyl benzanilide, water and hydrochloric acid are added in common response kettle, is heated up
To 30 DEG C, quick stirring 30 minutes, obtain dispersion liquid；
2）Diazo-reaction：Under acid condition, to step 1 at a temperature of -10 DEG C～10 DEG C）In the dispersion liquid for obtaining, 2-5 minute
Interior addition sodium nitrite in aqueous solution, carries out adding sodium acetate after diazo-reaction is stirred 60 minutes, that emulsifying agent obtains diazotising is molten
Liquid, the 3- amino-4-methoxyl benzanilide are 1 with emulsifying agent mass ratio：0.01 ~ 0.06, emulsifying agent is MOA-4；
3）Water, liquid caustic soda, chaotropic agent are added in dissolving reactor, 85-90 DEG C under stirring, is warming up to, add apthol AS-LC stirring
Flocculoreaction liquid is obtained, chaotropic agent is the one kind in alcohol, MOA-4, OS-15 or detergent 209, apthol AS-LC and chaotropic agent
Mass ratio be 1：0.02~0.1；
4）Coupling reaction：Controlling reaction temperature at 0 DEG C～15 DEG C, by step 3）Add in the settled solution 30-60 minute for obtaining
Step 2）Coupling reaction kettle in carry out coupling reaction, it is 5.5-6 to control reaction pH with 5% hydrochloric acid in course of reaction, and is incubated and stirs
Mix 1 ~ 2 hour and terminate to reaction；
5）Post processing：To step 4）Coupling reaction kettle in the clear rosin liquid of additionization, plus rosin liquid time control divides in 1-10
In clock；
6）Heat up and turn brilliant reaction：By step 5）Reactant liquor, be warming up to 70 ~ 100 DEG C, insulation reaction 30 minutes, then be down to room temperature,
Filter, dry at 80 ~ 110 DEG C and obtain solvent inkjet ink transparent type high glaze pigment red 146.
2. a kind of solvent inkjet ink according to claim 1 industrialized preparing process of transparent type high glaze pigment red 146, its
It is characterised by step 3）Described liquid caustic soda：Apthol AS-LC mol ratio is 1-3：1.
3. a kind of solvent inkjet ink according to claim 1 industrialized preparing process of transparent type high glaze pigment red 146, its
It is characterised by step 3）Described apthol AS-LC：Liquid caustic soda mol ratio is 1：2-3.
4. a kind of solvent inkjet ink according to claim 1 industrialized preparing process of transparent type high glaze pigment red 146, its
It is characterised by step 5）It is 70～100 DEG C that described post processing heats up.
5. a kind of solvent inkjet ink according to claim 1 industrialized preparing process of transparent type high glaze pigment red 146, its
It is characterised by step 5）Described apthol AS-LC：The mass ratio of rosin is 1：0.02～0.1.
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| CN109825105B (en) * | 2019-03-27 | 2020-11-10 | 山东宇虹新颜料股份有限公司 | Method for preparing nano-scale pigment red 146 by inverse miniemulsion method |
| CN110041725A (en) * | 2019-04-30 | 2019-07-23 | 江苏彩瑞实业有限公司 | A kind of technical process producing high light-fast fastness, high durable fastness pigment red 146 |
| CN110283475B (en) * | 2019-07-19 | 2021-06-01 | 杭州红妍颜料化工有限公司 | Preparation method of pigment red 146 |
| CN113105751B (en) * | 2021-04-15 | 2023-02-28 | 浙江科隆颜料科技有限公司 | Method for processing low aniline pigment diazo component |
| CN114085543B (en) * | 2021-11-17 | 2023-11-07 | 龙口联合化学股份有限公司 | Application of quaternary ammonium salt derivative in preparation of red pigment, red pigment and preparation method |
| CN116496636A (en) * | 2023-04-25 | 2023-07-28 | 宁夏保隆科技有限公司 | Synthesis process of acid yellow |
Citations (2)
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|---|---|---|---|---|
| CN101942217A (en) * | 2010-07-28 | 2011-01-12 | 吴江市屯村颜料厂 | Preparation method for special pigment for aqueous printing ink |
| CN104130590A (en) * | 2014-07-25 | 2014-11-05 | 嘉兴科隆化工有限公司 | Industrial production method for migration-resistant bright red pigment 150 used for PU |
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2014
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101942217A (en) * | 2010-07-28 | 2011-01-12 | 吴江市屯村颜料厂 | Preparation method for special pigment for aqueous printing ink |
| CN104130590A (en) * | 2014-07-25 | 2014-11-05 | 嘉兴科隆化工有限公司 | Industrial production method for migration-resistant bright red pigment 150 used for PU |
Non-Patent Citations (1)
| Title |
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| C.I.颜料红48:2的合成及改性研究;吕东军;《中国优秀博硕士学位论文全文数据库(硕士)工程科技Ⅰ辑》;20060615(第6期);论文正文第44页 * |
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Address after: The new road bridge Nanhu District town of Jiaxing City, Zhejiang province 314004 No. 268 Patentee after: Zhejiang Kelong pigment Technology Co., Ltd. Address before: The new road bridge Nanhu District town of Jiaxing city of Zhejiang Province in 314004 Patentee before: Crown Chemical Co., Ltd. |
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Denomination of invention: Industrial production method of transparent high-gloss pigment red 146 applied to solvent ink Effective date of registration: 20190724 Granted publication date: 20170308 Pledgee: Agricultural Bank of China Limited by Share Ltd Jiaxing science and Technology Branch Pledgor: Zhejiang Kelong pigment Technology Co., Ltd. Registration number: 2019330000206 |
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