CN102321380A - Method for preparing high-hiding variety paratonere 2BL of paratonere 177 - Google Patents
Method for preparing high-hiding variety paratonere 2BL of paratonere 177 Download PDFInfo
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Abstract
The invention relates to a method for preparing high-hiding variety paratonere 2BL of paratonere 177, which is characterized in that the bromamine acid condensation reaction comprises the steps that: 3800 parts of water and 30 parts of 98 percent sulphuric acid are introduced into a 5000 L condensation reaction kettle, then, 400 parts of bromamine acid is added, the temperature is raised to 85 to 90 DEG C, 100 parts of calcined soda is added slowly while the materials are hot, the stirring is carried out for 15 minutes, copper powder is filtered out, the filtering liquid is heated to 80 DEG C, 400 parts of sodium chloride is added for carrying out salting-out, the filtering is carried out when the temperature is lowered to 60 DEG C, a filter cake is washed by 4000 parts of 2 percent sodium chloride solution, condensation reaction crude products are obtained, the condensation reaction crude products are added into 4000 parts of hot water with the temperature being 85 to 90 DEG C and are dissolved through stirring, the filter liquid is then salted out by 400 parts of sodium chloride, the filtering is carried out when the temperature is lowered to 60 DEG C, the filter cake is washed by 4000 parts of 2 percent sodium chloride solution, and red brown condensation reaction fine products are obtained. The method has the advantages of high hiding, high tinctorial strength, high hydrothermal stability and easy dispersivity.
Description
Technical field
The invention belongs to the fine chemical technology field, relate in particular to the preparation method of a kind of a kind of high covering power kind Pigment red 2BL of Pigment red 177.
Background technology
Pigment red 2BL: English name, pigment call number: C.I.Pigment Red 177.Its structural formula is:
Main physical and chemical is:
Photostabilization: 7-8 level thermotolerance: 250 ℃
Acid resistance: 4 grades of alkali resistances: 5 grades
Water tolerance: 5 grades of solvent resistances: 5 grades
Oil-proofness: 5 grades of water solvent property: insoluble
Specific density: 1.45～1.53 tap densities: (lb/gal) 12.1～12.7
Specific surface area:! 65～106 fusing points of ㎡/g): (℃) 350
PH value: (10% slurry) 7.0～7.2 opacifying powers: high covering power
It is that blue light is red, lovely luster, and high covering power, tinting strength is high, and weather resisteant is strong, acid and alkali-resistance, heatproof reaches 250 ℃.Be mainly used in industrial coating, car paint, plastics painted.
The production technique of Pigment red 2BL is that raw material takes off sulphur pigmenting system through condensation with the bromamine acid at present, its reaction equation:
(1) condensation reaction:
(2) take off the sulphur reaction:
Summary of the invention
The purpose of this invention is to provide the preparation method of a kind of a kind of high covering power kind Pigment red 2BL of Pigment red 177, have very high opacifying power and dispersiveness, and coloured light is bright-coloured, excellent performance.
The technical scheme that the present invention adopts is:
The preparation method of a kind of high covering power kind Pigment red 2BL of Pigment red 177 comprises the condensation reaction of bromamine acid, the pigmenting processing of taking off sulphur reaction and bullion pigment of condenses;
The step of the condensation reaction of said bromamine acid: with the copper powder activation; 20% the dilute sulphuric acid that in the enamel reaction still of 500L, adds 400 parts starts stirring, slowly 200 parts copper powder is all added at leisure then; Be heated to 40-50 ℃ then; Stirred 30 minutes, filtered water is washed till neutrality, and the activation of copper powder is accomplished; In the condensation reaction still of 5000L, feed earlier 98% sulfuric acid of 3800 parts water and 30 parts, add 400 parts bromamine acid then, be warmed up to 85-90 ℃; Treat that bromamine acid dissolving adds activatory copper powder after transparent, insulation reaction 3 hours slowly adds 100 parts soda ash while hot; Stirred 15 minutes, and filtered the elimination copper powder; Filtrating is heated to 80 ℃, and the sodium-chlor that adds 400 parts is saltoutd, and filters when being cooled to 60 ℃; Filter cake is with the washing of 4000 part 2% sodium chloride solution, the condensation reaction crude product, the condensation reaction crude product is added in 4000 parts 85-90 ℃ the hot water; Stirring and dissolving, the charcoal absorption that adds 100 parts is filtered, and filtrating is saltoutd with 400 parts sodium-chlor again; Filter when being cooled to 60 ℃, filter cake is with 4000 part 2% sodium chloride solution washing, red-brown condensation reaction essence product (4.4 '-diaminostilbene .1 '-DIANTHRAQUINONE-3.3 '-disulfonic acid);
The step of taking off sulphur reaction of said condenses: 85% the sulfuric acid that in the enamel reaction still of 5000L, adds 3000 parts; Then the smart product of condensation reaction is added, temperature is controlled at 130-140 ℃ and reacted 3-5 hour down, with thin-layer chromatography detection reaction terminal point; Reaction finishes and is cooled to 70-90 ℃; To take off in the mixture of ice and water that iodine solution slowly joins 10000 parts, filter, filter cake with 2% sodium hydroxide solution washing to neutrality; Washed again 1 hour, the wine-colored sulphur product (4.4 '-diaminostilbene .1 '-DIANTHRAQUINONE) that take off;
Add in the enamel reaction still of the band condensing surface of the pigmenting processed steps of said bullion pigment: 10000L 500 parts take off sulphur product wet cake, 5-15 part dispersion agent and 5-15 part emulsifying agent, stirs after 3-4 hour, adding 1500 parts again must organic solvent; Reflux was reacted after 3-5 hour, and chuck is cooled to 30-35 ℃; The entrance pressure filter filters; Collect the filtrating recycling use, the filter cake washing is sent into baking oven after 2 hours and is carried out drying, promptly gets red anthraquinone reduction type pigment dyestuff.
Said organic solvent is a kind of in N-Methyl pyrrolidone, N, dinethylformamide, formic acid, acetate, chlorobenzene or the dichlorobenzene.
Said dispersion agent is an AEO silane, and said emulsifying agent is an alkyl phenol ethylene oxide condensate.
Advantage of the present invention is: high covering power, high tinting strength, high heat-resistant stability and easily disperse.
Embodiment
Embodiment 1
The preparation method of a kind of high covering power kind Pigment red 2BL of Pigment red 177 of the present invention comprises the condensation reaction of bromamine acid, the pigmenting processing of taking off sulphur reaction and bullion pigment of condenses;
The step of the condensation reaction of bromamine acid: with the copper powder activation; 20% the dilute sulphuric acid that in the enamel reaction still of 500L, adds 400 parts starts stirring, slowly 200 parts copper powder is all added at leisure then; Be heated to 40 ℃ then; Stirred 30 minutes, filtered water is washed till neutrality, and the activation of copper powder is accomplished; In the condensation reaction still of 5000L, feed earlier 98% sulfuric acid of 3800 parts water and 30 parts, add 400 parts bromamine acid then, be warmed up to 85 ℃; Treat that bromamine acid dissolving adds activatory copper powder after transparent, insulation reaction 3 hours slowly adds 100 parts soda ash while hot; Stirred 15 minutes, and filtered the elimination copper powder; Filtrating is heated to 80 ℃, and the sodium-chlor that adds 400 parts is saltoutd, and filters when being cooled to 60 ℃; Filter cake is with the washing of 4000 part 2% sodium chloride solution, the condensation reaction crude product, the condensation reaction crude product is added in 4000 parts 85 ℃ the hot water; Stirring and dissolving, the charcoal absorption that adds 100 parts is filtered, and filtrating is saltoutd with 400 parts sodium-chlor again; Filter when being cooled to 60 ℃, filter cake is with 4000 part 2% sodium chloride solution washing, red-brown condensation reaction essence product (4.4 '-diaminostilbene .1 '-DIANTHRAQUINONE-3.3 '-disulfonic acid);
The step of taking off sulphur reaction of condenses: 85% the sulfuric acid that in the enamel reaction still of 5000L, adds 3000 parts; Then the smart product of condensation reaction is added, temperature is controlled at 130 ℃ and reacted 3 hours down, with thin-layer chromatography detection reaction terminal point; Reaction finishes and is cooled to 70 ℃; To take off in the mixture of ice and water that iodine solution slowly joins 10000 parts, filter, filter cake with 2% sodium hydroxide solution washing to neutrality; Washed again 1 hour, the wine-colored sulphur product (4.4 '-diaminostilbene .1 '-DIANTHRAQUINONE) that take off;
Add in the enamel reaction still of the band condensing surface of the pigmenting processed steps of bullion pigment: 10000L 500 parts take off sulphur product wet cake, 5 parts of branch AEO silane and 5 parts of alkyl phenol ethylene oxide condensates; Stir after 3 hours, add 1500 parts again and get N-Methyl pyrrolidone, reflux; React after 3 hours; Chuck is cooled to 30 ℃, and the entrance pressure filter filters, and collects the filtrating recycling use; The filter cake washing is sent into baking oven after 2 hours and is carried out drying, promptly gets red anthraquinone reduction type pigment dyestuff.
Embodiment 2
The preparation method of a kind of high covering power kind Pigment red 2BL of Pigment red 177 comprises the condensation reaction of bromamine acid, the pigmenting processing of taking off sulphur reaction and bullion pigment of condenses;
The step of the condensation reaction of bromamine acid: with the copper powder activation; 20% the dilute sulphuric acid that in the enamel reaction still of 500L, adds 400 parts starts stirring, slowly 200 parts copper powder is all added at leisure then; Be heated to 42 ℃ then; Stirred 30 minutes, filtered water is washed till neutrality, and the activation of copper powder is accomplished; In the condensation reaction still of 5000L, feed earlier 98% sulfuric acid of 3800 parts water and 30 parts, add 400 parts bromamine acid then, be warmed up to 86 ℃; Treat that bromamine acid dissolving adds activatory copper powder after transparent, insulation reaction 3 hours slowly adds 100 parts soda ash while hot; Stirred 15 minutes, and filtered the elimination copper powder; Filtrating is heated to 80 ℃, and the sodium-chlor that adds 400 parts is saltoutd, and filters when being cooled to 60 ℃; Filter cake is with the washing of 4000 part 2% sodium chloride solution, the condensation reaction crude product, the condensation reaction crude product is added in 4000 parts 87 ℃ the hot water; Stirring and dissolving, the charcoal absorption that adds 100 parts is filtered, and filtrating is saltoutd with 400 parts sodium-chlor again; Filter when being cooled to 60 ℃, filter cake is with 4000 part 2% sodium chloride solution washing, red-brown condensation reaction essence product (4.4 '-diaminostilbene .1 '-DIANTHRAQUINONE-3.3 '-disulfonic acid);
The step of taking off sulphur reaction of condenses: 85% the sulfuric acid that in the enamel reaction still of 5000L, adds 3000 parts; Then the smart product of condensation reaction is added, temperature is controlled at 132 ℃ and reacted 3-5 hour down, with thin-layer chromatography detection reaction terminal point; Reaction finishes and is cooled to 75 ℃; To take off in the mixture of ice and water that iodine solution slowly joins 10000 parts, filter, filter cake with 2% sodium hydroxide solution washing to neutrality; Washed again 1 hour, the wine-colored sulphur product (4.4 '-diaminostilbene .1 '-DIANTHRAQUINONE) that take off;
Add in the enamel reaction still of the band condensing surface of the pigmenting processed steps of bullion pigment: 10000L 500 parts take off sulphur product wet cake, 7 parts of branch AEO silane and 7 parts of alkyl phenol ethylene oxide condensates; Stir after 3.5 hours, add 1500 parts again and get N, dinethylformamide, reflux; React after 4 hours; Chuck is cooled to 31 ℃, and the entrance pressure filter filters, and collects the filtrating recycling use; The filter cake washing is sent into baking oven after 2 hours and is carried out drying, promptly gets red anthraquinone reduction type pigment dyestuff.
Embodiment 3
The preparation method of a kind of high covering power kind Pigment red 2BL of Pigment red 177 comprises the condensation reaction of bromamine acid, the pigmenting processing of taking off sulphur reaction and bullion pigment of condenses;
The step of the condensation reaction of bromamine acid: with the copper powder activation; 20% the dilute sulphuric acid that in the enamel reaction still of 500L, adds 400 parts starts stirring, slowly 200 parts copper powder is all added at leisure then; Be heated to 44 ℃ then; Stirred 30 minutes, filtered water is washed till neutrality, and the activation of copper powder is accomplished; In the condensation reaction still of 5000L, feed earlier 98% sulfuric acid of 3800 parts water and 30 parts, add 400 parts bromamine acid then, be warmed up to 87 ℃; Treat that bromamine acid dissolving adds activatory copper powder after transparent, insulation reaction 3 hours slowly adds 100 parts soda ash while hot; Stirred 15 minutes, and filtered the elimination copper powder; Filtrating is heated to 80 ℃, and the sodium-chlor that adds 400 parts is saltoutd, and filters when being cooled to 60 ℃; Filter cake is with the washing of 4000 part 2% sodium chloride solution, the condensation reaction crude product, the condensation reaction crude product is added in 4000 parts 88 ℃ the hot water; Stirring and dissolving, the charcoal absorption that adds 100 parts is filtered, and filtrating is saltoutd with 400 parts sodium-chlor again; Filter when being cooled to 60 ℃, filter cake is with 4000 part 2% sodium chloride solution washing, red-brown condensation reaction essence product (4.4 '-diaminostilbene .1 '-DIANTHRAQUINONE-3.3 '-disulfonic acid);
The step of taking off sulphur reaction of condenses: 85% the sulfuric acid that in the enamel reaction still of 5000L, adds 3000 parts; Then the smart product of condensation reaction is added, temperature is controlled at 134 ℃ and reacted 3 hours down, with thin-layer chromatography detection reaction terminal point; Reaction finishes and is cooled to 80 ℃; To take off in the mixture of ice and water that iodine solution slowly joins 10000 parts, filter, filter cake with 2% sodium hydroxide solution washing to neutrality; Washed again 1 hour, the wine-colored sulphur product (4.4 '-diaminostilbene .1 '-DIANTHRAQUINONE) that take off;
Add in the enamel reaction still of the band condensing surface of the pigmenting processed steps of bullion pigment: 10000L 500 parts take off sulphur product wet cake, 10 parts of branch AEO silane and 10 parts of alkyl phenol ethylene oxide condensates; Stir after 3 hours, add 1500 parts again and get formic acid, reflux; React after 4 hours; Chuck is cooled to 33 ℃, and the entrance pressure filter filters, and collects the filtrating recycling use; The filter cake washing is sent into baking oven after 2 hours and is carried out drying, promptly gets red anthraquinone reduction type pigment dyestuff.
Embodiment 4
The preparation method of a kind of high covering power kind Pigment red 2BL of Pigment red 177 comprises the condensation reaction of bromamine acid, the pigmenting processing of taking off sulphur reaction and bullion pigment of condenses;
The step of the condensation reaction of bromamine acid: with the copper powder activation; 20% the dilute sulphuric acid that in the enamel reaction still of 500L, adds 400 parts starts stirring, slowly 200 parts copper powder is all added at leisure then; Be heated to 46 ℃ then; Stirred 30 minutes, filtered water is washed till neutrality, and the activation of copper powder is accomplished; In the condensation reaction still of 5000L, feed earlier 98% sulfuric acid of 3800 parts water and 30 parts, add 400 parts bromamine acid then, be warmed up to 89 ℃; Treat that bromamine acid dissolving adds activatory copper powder after transparent, insulation reaction 3 hours slowly adds 100 parts soda ash while hot; Stirred 15 minutes, and filtered the elimination copper powder; Filtrating is heated to 80 ℃, and the sodium-chlor that adds 400 parts is saltoutd, and filters when being cooled to 60 ℃; Filter cake is with the washing of 4000 part 2% sodium chloride solution, the condensation reaction crude product, the condensation reaction crude product is added in 4000 parts 88 ℃ the hot water; Stirring and dissolving, the charcoal absorption that adds 100 parts is filtered, and filtrating is saltoutd with 400 parts sodium-chlor again; Filter when being cooled to 60 ℃, filter cake is with 4000 part 2% sodium chloride solution washing, red-brown condensation reaction essence product (4.4 '-diaminostilbene .1 '-DIANTHRAQUINONE-3.3 '-disulfonic acid);
The step of taking off sulphur reaction of condenses: 85% the sulfuric acid that in the enamel reaction still of 5000L, adds 3000 parts; Then the smart product of condensation reaction is added, temperature is controlled at 137 ℃ and reacted 3.5 hours down, with thin-layer chromatography detection reaction terminal point; Reaction finishes and is cooled to 88 ℃; To take off in the mixture of ice and water that iodine solution slowly joins 10000 parts, filter, filter cake with 2% sodium hydroxide solution washing to neutrality; Washed again 1 hour, the wine-colored sulphur product (4.4 '-diaminostilbene .1 '-DIANTHRAQUINONE) that take off;
Add in the enamel reaction still of the band condensing surface of the pigmenting processed steps of bullion pigment: 10000L 500 parts take off sulphur product wet cake, 12 parts of branch AEO silane and 12 parts of alkyl phenol ethylene oxide condensates; Stir after 3.5 hours, add 1500 parts again and get acetate, reflux; React after 4 hours; Chuck is cooled to 34 ℃, and the entrance pressure filter filters, and collects the filtrating recycling use; The filter cake washing is sent into baking oven after 2 hours and is carried out drying, promptly gets red anthraquinone reduction type pigment dyestuff.
Embodiment 5
The preparation method of a kind of high covering power kind Pigment red 2BL of Pigment red 177 comprises the condensation reaction of bromamine acid, the pigmenting processing of taking off sulphur reaction and bullion pigment of condenses;
The step of the condensation reaction of bromamine acid: with the copper powder activation; 20% the dilute sulphuric acid that in the enamel reaction still of 500L, adds 400 parts starts stirring, slowly 200 parts copper powder is all added at leisure then; Be heated to 48 ℃ then; Stirred 30 minutes, filtered water is washed till neutrality, and the activation of copper powder is accomplished; In the condensation reaction still of 5000L, feed earlier 98% sulfuric acid of 3800 parts water and 30 parts, add 400 parts bromamine acid then, be warmed up to 89 ℃; Treat that bromamine acid dissolving adds activatory copper powder after transparent, insulation reaction 3 hours slowly adds 100 parts soda ash while hot; Stirred 15 minutes, and filtered the elimination copper powder; Filtrating is heated to 80 ℃, and the sodium-chlor that adds 400 parts is saltoutd, and filters when being cooled to 60 ℃; Filter cake is with the washing of 4000 part 2% sodium chloride solution, the condensation reaction crude product, the condensation reaction crude product is added in 4000 parts 89 ℃ the hot water; Stirring and dissolving, the charcoal absorption that adds 100 parts is filtered, and filtrating is saltoutd with 400 parts sodium-chlor again; Filter when being cooled to 60 ℃, filter cake is with 4000 part 2% sodium chloride solution washing, red-brown condensation reaction essence product (4.4 '-diaminostilbene .1 '-DIANTHRAQUINONE-3.3 '-disulfonic acid);
The step of taking off sulphur reaction of condenses: 85% the sulfuric acid that in the enamel reaction still of 5000L, adds 3000 parts; Then the smart product of condensation reaction is added, temperature is controlled at 138 ℃ and reacted 4.5 hours down, with thin-layer chromatography detection reaction terminal point; Reaction finishes and is cooled to 78 ℃; To take off in the mixture of ice and water that iodine solution slowly joins 10000 parts, filter, filter cake with 2% sodium hydroxide solution washing to neutrality; Washed again 1 hour, the wine-colored sulphur product (4.4 '-diaminostilbene .1 '-DIANTHRAQUINONE) that take off;
Add in the enamel reaction still of the band condensing surface of the pigmenting processed steps of bullion pigment: 10000L 500 parts take off sulphur product wet cake, 14 parts of branch AEO silane and 14 parts of alkyl phenol ethylene oxide condensates; Stir after 4 hours, add 1500 parts again and get chlorobenzene, reflux; React after 5 hours; Chuck is cooled to 34 ℃, and the entrance pressure filter filters, and collects the filtrating recycling use; The filter cake washing is sent into baking oven after 2 hours and is carried out drying, promptly gets red anthraquinone reduction type pigment dyestuff.
Embodiment 6
The preparation method of a kind of high covering power kind Pigment red 2BL of Pigment red 177 comprises the condensation reaction of bromamine acid, the pigmenting processing of taking off sulphur reaction and bullion pigment of condenses;
The step of the condensation reaction of bromamine acid: with the copper powder activation; 20% the dilute sulphuric acid that in the enamel reaction still of 500L, adds 400 parts starts stirring, slowly 200 parts copper powder is all added at leisure then; Be heated to 50 ℃ then; Stirred 30 minutes, filtered water is washed till neutrality, and the activation of copper powder is accomplished; In the condensation reaction still of 5000L, feed earlier 98% sulfuric acid of 3800 parts water and 30 parts, add 400 parts bromamine acid then, be warmed up to 90 ℃; Treat that bromamine acid dissolving adds activatory copper powder after transparent, insulation reaction 3 hours slowly adds 100 parts soda ash while hot; Stirred 15 minutes, and filtered the elimination copper powder; Filtrating is heated to 80 ℃, and the sodium-chlor that adds 400 parts is saltoutd, and filters when being cooled to 60 ℃; Filter cake is with the washing of 4000 part 2% sodium chloride solution, the condensation reaction crude product, the condensation reaction crude product is added in 4000 parts 90 ℃ the hot water; Stirring and dissolving, the charcoal absorption that adds 100 parts is filtered, and filtrating is saltoutd with 400 parts sodium-chlor again; Filter when being cooled to 60 ℃, filter cake is with 4000 part 2% sodium chloride solution washing, red-brown condensation reaction essence product (4.4 '-diaminostilbene .1 '-DIANTHRAQUINONE-3.3 '-disulfonic acid);
The step of taking off sulphur reaction of condenses: 85% the sulfuric acid that in the enamel reaction still of 5000L, adds 3000 parts; Then the smart product of condensation reaction is added, temperature is controlled at 140 ℃ and reacted 5 hours down, with thin-layer chromatography detection reaction terminal point; Reaction finishes and is cooled to 90 ℃; To take off in the mixture of ice and water that iodine solution slowly joins 10000 parts, filter, filter cake with 2% sodium hydroxide solution washing to neutrality; Washed again 1 hour, the wine-colored sulphur product (4.4 '-diaminostilbene .1 '-DIANTHRAQUINONE) that take off;
Add in the enamel reaction still of the band condensing surface of the pigmenting processed steps of bullion pigment: 10000L 500 parts take off sulphur product wet cake, 15 parts of branch AEO silane and 15 parts of alkyl phenol ethylene oxide condensates; Stir after 4 hours, add 1500 parts again and get dichlorobenzene, reflux; React after 5 hours; Chuck is cooled to 35 ℃, and the entrance pressure filter filters, and collects the filtrating recycling use; The filter cake washing is sent into baking oven after 2 hours and is carried out drying, promptly gets red anthraquinone reduction type pigment dyestuff.
Claims (3)
1. the preparation method of a kind of high covering power kind Pigment red 2BL of Pigment red 177 is characterized in that:
Comprise the condensation reaction of bromamine acid, the pigmenting processing of taking off sulphur reaction and bullion pigment of condenses;
The step of the condensation reaction of said bromamine acid: with the copper powder activation; 20% the dilute sulphuric acid that in the enamel reaction still of 500L, adds 400 parts starts stirring, slowly 200 parts copper powder is all added at leisure then; Be heated to 40-50 ℃ then; Stirred 30 minutes, filtered water is washed till neutrality, and the activation of copper powder is accomplished; In the condensation reaction still of 5000L, feed earlier 98% sulfuric acid of 3800 parts water and 30 parts, add 400 parts bromamine acid then, be warmed up to 85-90 ℃; Treat that bromamine acid dissolving adds activatory copper powder after transparent, insulation reaction 3 hours slowly adds 100 parts soda ash while hot; Stirred 15 minutes, and filtered the elimination copper powder; Filtrating is heated to 80 ℃, and the sodium-chlor that adds 400 parts is saltoutd, and filters when being cooled to 60 ℃; Filter cake is with the washing of 4000 part 2% sodium chloride solution, the condensation reaction crude product, the condensation reaction crude product is added in 4000 parts 85-90 ℃ the hot water; Stirring and dissolving, the charcoal absorption that adds 100 parts is filtered, and filtrating is saltoutd with 400 parts sodium-chlor again; Filter when being cooled to 60 ℃, filter cake is with 4000 part 2% sodium chloride solution washing, red-brown condensation reaction essence product (4.4 '-diaminostilbene .1 '-DIANTHRAQUINONE-3.3 '-disulfonic acid);
The step of taking off sulphur reaction of said condenses: 85% the sulfuric acid that in the enamel reaction still of 5000L, adds 3000 parts; Then the smart product of condensation reaction is added, temperature is controlled at 130-140 ℃ and reacted 3-5 hour down, with thin-layer chromatography detection reaction terminal point; Reaction finishes and is cooled to 70-90 ℃; To take off in the mixture of ice and water that iodine solution slowly joins 10000 parts, filter, filter cake with 2% sodium hydroxide solution washing to neutrality; Washed again 1 hour, the wine-colored sulphur product (4.4 '-diaminostilbene .1 '-DIANTHRAQUINONE) that take off;
Add in the enamel reaction still of the band condensing surface of the pigmenting processed steps of said bullion pigment: 10000L 500 parts take off sulphur product wet cake, 5-15 part dispersion agent and 5-15 part emulsifying agent, stirs after 3-4 hour, adding 1500 parts again must organic solvent; Reflux was reacted after 3-5 hour, and chuck is cooled to 30-35 ℃; The entrance pressure filter filters; Collect the filtrating recycling use, the filter cake washing is sent into baking oven after 2 hours and is carried out drying, promptly gets red anthraquinone reduction type pigment dyestuff.
2. the preparation method of a kind of high covering power kind Pigment red 2BL of Pigment red 177 according to claim 1 is characterized in that: said organic solvent is a kind of in N-Methyl pyrrolidone, N, dinethylformamide, formic acid, acetate, chlorobenzene or the dichlorobenzene.
3. the preparation method of a kind of high covering power kind Pigment red 2BL of Pigment red 177 according to claim 1, it is characterized in that: said dispersion agent is an AEO silane, said emulsifying agent is an alkyl phenol ethylene oxide condensate.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103773079A (en) * | 2014-02-25 | 2014-05-07 | 山东宇虹新颜料股份有限公司 | Method for preparing pigment red 177 in ionic liquid |
| CN106084884A (en) * | 2016-06-12 | 2016-11-09 | 南通市争妍颜料化工有限公司 | Pigment red 3 BL pigmentation processes technique |
| CN107459470A (en) * | 2017-08-25 | 2017-12-12 | 天津城建大学 | The method that heterogeneous system catalyzes and synthesizes bromamine acid condensation product |
| CN109704979A (en) * | 2019-01-29 | 2019-05-03 | 山东宇虹新颜料股份有限公司 | 4,4- diaminostilbene, the method for 1- dianthraquinone are efficiently prepared using Bronsted acidic functionalized ionic liquid |
| CN115011138A (en) * | 2022-05-18 | 2022-09-06 | 宁夏彩妍科技有限公司 | Production method and production system of pigment red 177 for liquid crystal display screen |
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| 任东文: "颜料分散型液晶彩色显示用聚酰亚胺滤色片材料的研制", 《大连理工大学 硕士学位论文》 * |
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| CN103773079A (en) * | 2014-02-25 | 2014-05-07 | 山东宇虹新颜料股份有限公司 | Method for preparing pigment red 177 in ionic liquid |
| CN103773079B (en) * | 2014-02-25 | 2016-02-17 | 山东宇虹新颜料股份有限公司 | The method of Pigment red 177 is prepared in ionic liquid |
| CN106084884A (en) * | 2016-06-12 | 2016-11-09 | 南通市争妍颜料化工有限公司 | Pigment red 3 BL pigmentation processes technique |
| CN107459470A (en) * | 2017-08-25 | 2017-12-12 | 天津城建大学 | The method that heterogeneous system catalyzes and synthesizes bromamine acid condensation product |
| CN109704979A (en) * | 2019-01-29 | 2019-05-03 | 山东宇虹新颜料股份有限公司 | 4,4- diaminostilbene, the method for 1- dianthraquinone are efficiently prepared using Bronsted acidic functionalized ionic liquid |
| CN109704979B (en) * | 2019-01-29 | 2022-01-21 | 山东宇虹新颜料股份有限公司 | Method for efficiently preparing 4, 4-diamino-1, 1-dianthraquinone by using Bronsted acid functionalized ionic liquid |
| CN115011138A (en) * | 2022-05-18 | 2022-09-06 | 宁夏彩妍科技有限公司 | Production method and production system of pigment red 177 for liquid crystal display screen |
| CN115011138B (en) * | 2022-05-18 | 2023-11-17 | 宁夏彩妍科技有限公司 | Production method and production system of pigment red 177 for liquid crystal display screen |
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