CN105694523A - Preparation method of disperse blue - Google Patents
Preparation method of disperse blue Download PDFInfo
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- CN105694523A CN105694523A CN201610057984.6A CN201610057984A CN105694523A CN 105694523 A CN105694523 A CN 105694523A CN 201610057984 A CN201610057984 A CN 201610057984A CN 105694523 A CN105694523 A CN 105694523A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B43/00—Preparation of azo dyes from other azo compounds
- C09B43/40—Preparation of azo dyes from other azo compounds by substituting hetero atoms by radicals containing other hetero atoms
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Abstract
The invention relates to a preparation method of disperse blue. The method comprises the following steps: (1) in a DMF (N,N-dimethylformamide) solvent, adding cuprous cyanide, adding sodium cyanide or zinc cyanide, and carrying out complexation to obtain a complex solution; (2) adding N-(2-((2,6-dibromo-4-nitrophenyl)azo)-5-(diethylamino)phenyl)acetamide into a DMF solvent, and dissolving by heating to obtain a filter cake solution; (3) slowly adding the complex solution into the filter cake solution, carrying out cyanation, cooling after the cyanation finishes, adding water to separate out cyanide, filtering, washing to obtain a disperse blue 165 coarse filter cake, mixing a mother solution and washing water, and adding sodium hyposulfite to remove toxins and recover the DMF; and (4) adding water, hydrochloric acid and ferric chloride into a toxic removal solution preparation pot to obtain a toxic removal solution, adding water and the disperse blue 165 coarse filter cake into a toxic removal pot, pulping, adding the toxic removal solution to perform toxic removal, filtering, and washing to obtain the disperse blue 165 filter cake. The method has the advantages of safe production technique, complete reaction, fewer side reactions and impurities, and high product quality.
Description
Technical field
The invention belongs to disperse dyes field, the preparation method of especially a kind of disperse blue。
Background technology
Disperse blue 165, is the disperse dyes of monoazo, can be used for the colorant match of the disperse blue such as disperse blue 2B, BBLS。Meeting copper, iron ion coloured light during dyeing all unchanged, for the dyeing of terylene and blend fabric thereof, this dye shade is gorgeous, and lifting force is good, and temperature is more sensitive, and colouring curve is steeper。
The dominant response producing disperse blue 165 at present is as follows:
Acetamide is with DMF for solvent for N-(2-((the bromo-4-nitrobenzophenone of 2,6-bis-) azo)-5-(diethylamino) phenyl), with sodium bromide for catalyst, and Cupricin. reaction。During this explained hereafter, reaction temperature requires height, and response speed is relatively slow, and energy consumption is big, and product yield is relatively low, and side reaction and impurity are more；Production cost is higher, and production efficiency is relatively low。
Summary of the invention
Present invention aim to overcome that the deficiencies in the prior art, it is provided that a kind of production technology safety, react completely, side reaction and impurity are few, the preparation method of the disperse blue of good product quality。
The preparation method of a kind of disperse blue, comprises the steps:
(1), complexation:
Complexation pot adds DMF, Cupricin., Cyanogran. or zinc cyanide, is warmed up to 70 DEG C, 70～75 DEG C of stirring reactions 30 minutes, be cooled to 45～50 DEG C, obtain complex liquid；
(2), filter cake dissolves:
Cyaniding pot adds DMF, N-(2-((2,6-bis-bromo-4-nitrobenzophenone) azo)-5-(diethylamino) phenyl) acetamide, after stirring evenly, it is warmed up to 95～100 DEG C, is incubated 1 hour, it is cooled to 45～50 DEG C, obtains filter cake solution；
(3), cyaniding:
Complex liquid is slowly added in cyaniding pot filter cake solution, within 0.5～1 hour, add, temperature is maintained at 45～50 DEG C, 60～65 DEG C it are slowly ramped to after adding, insulation reaction 1 hour, it is slowly ramped to 80～85 DEG C again, insulation reaction 1 hour, survey terminal, if terminal arrives, then it is cooled to 30 DEG C, if terminal less than, it is warming up to 105～110 DEG C again, insulation reaction 1.5 hours, it is cooled to 30 DEG C, add 1000～1500kg water, add water 0.5～1 hour time, temperature is maintained at 20～30 DEG C, stir 10 minutes after adding, filter, filter cake 800kg water washing, obtain disperse blue 165 coarse filtration cake, mother liquid coming and washings mixing add 25kg sodium hyposulfite except poison recovery DMF；
(4), filter cake is except poison:
Preparing in pot except venom, adding water, hydrochloric acid, ferric chloride, stirring to dissolving except venom, then in removing poison pot, 5000kg water is added, put into disperse blue 165 coarse filtration cake, pull an oar 2～3 hours, after filter cake is broken up, add except venom, stir 12 hours, be fed to pressure filter, first wash to pH6.5～7 with room temperature water, then being colourless with 50～60 DEG C of water washings to washings, discharging obtains disperse blue 165 filter cake。
DMF described in described step (1): Cupricin.: the mass ratio of Cyanogran. is 4:1:0.53～0.54；DMF: Cupricin.: the mass ratio of zinc cyanide is 4:1:0.65。
The mass ratio of DMF, N-(2-((the bromo-4-nitrobenzophenone of 2,6-bis-) azo)-5-(diethylamino) phenyl) acetamide described in described step (2) is 2.5～3.5:1。
The mass ratio of the Cupricin. described in described step (3): N-(2-((the bromo-4-nitrobenzophenone of 2,6-bis-) azo)-5-(diethylamino) phenyl) acetamide is 1:5。
Water described in described step (4), hydrochloric acid, ferric chloride, disperse blue 165 coarse filtration cake mass ratio be 1～2:1:0.36～0.37:1。
Reaction equation:
(1) complexation
CuCN+NaCN→CUNa(CN)2
2CuCN+Zn(CN)2→Cu2Zn(CN)4
(2) cyaniding
(3) except poison
2CuNa(CN)2+2FeCl3→Na2Fe(CN)4+2CuCl2+FeCl2
CuZn(CN)4+2FeCl3→ZnFe(CN)4+2CuCl2+FeCl2
Compared with prior art, beneficial effects of the present invention is embodied in:
(1), the method that adopts Cupricin. and Cyanogran. or zinc cyanide compound cyanidization agent, cyaniding ability is strong, and reaction condition is gentle, and reaction is fast, reacts completely, and side reaction and impurity are few, good product quality。
(2), cyaniding time adopt the cyanidization agent of dropping complexation, and adopt segmentation insulation reaction, can effectively reduce the generation of side reaction。
Detailed description of the invention:
Embodiment 1
(1), complexation:
Complexation pot adds 600kgDMF, 150kg Cupricin., 79.5kg Cyanogran., is warmed up to 70 DEG C, 70～75 DEG C of stirring reactions 30 minutes, be cooled to 45～50 DEG C, obtain complex liquid；
(2), filter cake dissolves:
Cyaniding pot adds 1875kgDMF, 750kgN-(2-((2, the bromo-4-nitrobenzophenone of 6-bis-) azo)-5-(diethylamino) phenyl) acetamide, after stirring evenly, it is warmed up to 95～100 DEG C, it is incubated 1 hour, is cooled to 45～50 DEG C, obtains filter cake solution；
(3), cyaniding:
Complex liquid is slowly added in cyaniding pot filter cake solution, within 0.5～1 hour, add, temperature is maintained at 45～50 DEG C, 60～65 DEG C it are slowly ramped to after adding, insulation reaction 1 hour, it is slowly ramped to 80～85 DEG C again, insulation reaction 1 hour, survey terminal, if terminal arrives, then it is cooled to 30 DEG C, if terminal less than, it is warming up to 105～110 DEG C again, insulation reaction 1.5 hours, it is cooled to 30 DEG C, add 1000kg water, add water 0.5～1 hour time, temperature is maintained at 20～30 DEG C, stir 10 minutes after adding, filter, filter cake 800kg water washing, obtain 550kg disperse blue 165 coarse filtration cake, mother liquid coming and washings mixing add 25kg sodium hyposulfite except poison recovery DMF；
(4), filter cake is except poison:
Preparing in pot except venom, add 550kg water, 550kg hydrochloric acid, 200kg ferric chloride, stir to dissolving except venom, then in removing poison pot, 5000kg water is added, put into 550kg disperse blue 165 coarse filtration cake, pull an oar 2～3 hours, after filter cake is broken up, add except venom, stir 12 hours, be fed to pressure filter, first wash to pH6.5～7 with room temperature water, then being colourless with 50～60 DEG C of water washings to washings, discharging obtains 530kg disperse blue 165 filter cake。
Embodiment 2
(1), complexation:
Complexation pot adds 600kgDMF, 150kg Cupricin., 97.5kg zinc cyanide, is warmed up to 70 DEG C, 70～75 DEG C of stirring reactions 30 minutes, be cooled to 45～50 DEG C, obtain complex liquid；
(2), filter cake dissolves:
Cyaniding pot adds 1875kgDMF, 750kgN-(2-((2, the bromo-4-nitrobenzophenone of 6-bis-) azo)-5-(diethylamino) phenyl) acetamide, after stirring evenly, it is warmed up to 95～100 DEG C, it is incubated 1 hour, is cooled to 45～50 DEG C, obtains filter cake solution；
(3), cyaniding:
Complex liquid is slowly added in cyaniding pot filter cake solution, within 0.5～1 hour, add, temperature is maintained at 45～50 DEG C, 60～65 DEG C it are slowly ramped to after adding, insulation reaction 1 hour, it is slowly ramped to 80～85 DEG C again, insulation reaction 1 hour, survey terminal, if terminal arrives, then it is cooled to 30 DEG C, if terminal less than, it is warming up to 105～110 DEG C again, insulation reaction 1.5 hours, it is cooled to 30 DEG C, add 1000kg water, add water 0.5～1 hour time, temperature is maintained at 20～30 DEG C, stir 10 minutes after adding, filter, filter cake 800kg water washing, obtain 555kg disperse blue 165 coarse filtration cake, mother liquid coming and washings mixing add 25kg sodium hyposulfite except poison recovery DMF；
(4), filter cake is except poison:
Preparing in pot except venom, add 555kg water, 555kg hydrochloric acid, 200kg ferric chloride, stir to dissolving except venom, then in removing poison pot, 5000kg water is added, put into disperse blue 165 coarse filtration cake, pull an oar 2～3 hours, after filter cake is broken up, add except venom, stir 12 hours, be fed to pressure filter, first wash to pH6.5～7 with room temperature water, then being colourless with 50～60 DEG C of water washings to washings, discharging obtains 540kg disperse blue 165 filter cake。
Embodiment 3
(1), complexation:
Complexation pot adds 600kgDMF, 150kg Cupricin., 80.5kg Cyanogran., is warmed up to 70 DEG C, 70～75 DEG C of stirring reactions 30 minutes, be cooled to 45～50 DEG C, obtain complex liquid；
(2), filter cake dissolves:
Cyaniding pot adds 2625kgDMF, 750kgN-(2-((2, the bromo-4-nitrobenzophenone of 6-bis-) azo)-5-(diethylamino) phenyl) acetamide, after stirring evenly, it is warmed up to 95～100 DEG C, it is incubated 1 hour, is cooled to 45～50 DEG C, obtains filter cake solution；
(3), cyaniding:
Complex liquid is slowly added in cyaniding pot filter cake solution, within 0.5～1 hour, add, temperature is maintained at 45～50 DEG C, 60～65 DEG C it are slowly ramped to after adding, insulation reaction 1 hour, it is slowly ramped to 80～85 DEG C again, insulation reaction 1 hour, survey terminal, if terminal arrives, then it is cooled to 30 DEG C, if terminal less than, it is warming up to 105～110 DEG C again, insulation reaction 1.5 hours, it is cooled to 30 DEG C, add 1500kg water, add water 0.5～1 hour time, temperature is maintained at 20～30 DEG C, stir 10 minutes after adding, filter, filter cake 800kg water washing, obtain 550kg disperse blue 165 coarse filtration cake, mother liquid coming and washings mixing add 25kg sodium hyposulfite except poison recovery DMF；
(4), filter cake is except poison:
Preparing in pot except venom, add 1100kg water, 550kg hydrochloric acid, 200kg ferric chloride, stir to dissolving except venom, then in removing poison pot, 5000kg water is added, put into disperse blue 165 coarse filtration cake, pull an oar 2～3 hours, after filter cake is broken up, add except venom, stir 12 hours, be fed to pressure filter, first wash to pH6.5～7 with room temperature water, then being colourless with 50～60 DEG C of water washings to washings, discharging obtains 545kg disperse blue 165 filter cake。
Embodiment 4
(1), complexation:
Complexation pot adds 600kgDMF, 150kg Cupricin., 97.5kg zinc cyanide, is warmed up to 70 DEG C, 70～75 DEG C of stirring reactions 30 minutes, be cooled to 45～50 DEG C, obtain complex liquid；
(2), filter cake dissolves:
Cyaniding pot adds 2000kgDMF, 750kgN-(2-((2, the bromo-4-nitrobenzophenone of 6-bis-) azo)-5-(diethylamino) phenyl) acetamide, after stirring evenly, it is warmed up to 95～100 DEG C, it is incubated 1 hour, is cooled to 45～50 DEG C, obtains filter cake solution；
(3), cyaniding:
Complex liquid is slowly added in cyaniding pot filter cake solution, within 0.5～1 hour, add, temperature is maintained at 45～50 DEG C, 60～65 DEG C it are slowly ramped to after adding, insulation reaction 1 hour, it is slowly ramped to 80～85 DEG C again, insulation reaction 1 hour, survey terminal, if terminal arrives, then it is cooled to 30 DEG C, if terminal less than, it is warming up to 105～110 DEG C again, insulation reaction 1.5 hours, it is cooled to 30 DEG C, add 1200kg water, add water 0.5～1 hour time, temperature is maintained at 20～30 DEG C, stir 10 minutes after adding, filter, filter cake 800kg water washing, obtain 550kg disperse blue 165 coarse filtration cake, mother liquid coming and washings mixing add 25kg sodium hyposulfite except poison recovery DMF；
(4), filter cake is except poison:
Preparing in pot except venom, add 800kg water, 550kg hydrochloric acid, 200kg ferric chloride, stir to dissolving except venom, then in removing poison pot, 5000kg water is added, put into disperse blue 165 coarse filtration cake, pull an oar 2～3 hours, after filter cake is broken up, add except venom, stir 12 hours, be fed to pressure filter, first wash to pH6.5～7 with room temperature water, then being colourless with 50～60 DEG C of water washings to washings, discharging obtains 535kg disperse blue 165 filter cake。
Claims (5)
1. the preparation method of a disperse blue, it is characterised in that: comprise the steps:
(1), complexation:
Complexation pot adds DMF, Cupricin., Cyanogran. or zinc cyanide, is warmed up to 70 DEG C, 70～75 DEG C of stirring reactions 30 minutes, be cooled to 45～50 DEG C, obtain complex liquid；
(2), filter cake dissolves:
Cyaniding pot adds DMF, N-(2-((2,6-bis-bromo-4-nitrobenzophenone) azo)-5-(diethylamino) phenyl) acetamide, after stirring evenly, it is warmed up to 95～100 DEG C, is incubated 1 hour, it is cooled to 45～50 DEG C, obtains filter cake solution；
(3), cyaniding:
Complex liquid is slowly added in cyaniding pot filter cake solution, within 0.5～1 hour, add, temperature is maintained at 45～50 DEG C, 60～65 DEG C it are slowly ramped to after adding, insulation reaction 1 hour, it is slowly ramped to 80～85 DEG C again, insulation reaction 1 hour, survey terminal, if terminal arrives, then it is cooled to 30 DEG C, if terminal less than, it is warming up to 105～110 DEG C again, insulation reaction 1.5 hours, it is cooled to 30 DEG C, add 1000～1500kg water, add water 0.5～1 hour time, temperature is maintained at 20～30 DEG C, stir 10 minutes after adding, filter, filter cake 800kg water washing, obtain disperse blue 165 coarse filtration cake, mother liquid coming and washings mixing add 25kg sodium hyposulfite except poison recovery DMF；
(4), filter cake is except poison:
Preparing in pot except venom, adding water, hydrochloric acid, ferric chloride, stirring to dissolving except venom, then in removing poison pot, 5000kg water is added, put into disperse blue 165 coarse filtration cake, pull an oar 2～3 hours, after filter cake is broken up, add except venom, stir 12 hours, be fed to pressure filter, first wash to pH6.5～7 with room temperature water, then being colourless with 50～60 DEG C of water washings to washings, discharging obtains disperse blue 165 filter cake。
2. the preparation method of a kind of disperse blue according to claim 1, it is characterised in that the DMF described in described step (1): Cupricin.: the mass ratio of Cyanogran. is 4:1:0.53～0.54；DMF: Cupricin.: the mass ratio of zinc cyanide is 4:1:0.65。
3. the preparation method of a kind of disperse blue according to claim 1, it is characterized in that, the mass ratio of DMF, N-(2-((2,6-bis-bromo-4-nitrobenzophenone) azo)-5-(diethylamino) phenyl) acetamide described in described step (2) is 2.5～3.5:1。
4. the preparation method of a kind of disperse blue according to claim 1, it is characterized in that, the mass ratio of the Cupricin. described in described step (3): N-(2-((2,6-bis-bromo-4-nitrobenzophenone) azo)-5-(diethylamino) phenyl) acetamide is 1:5。
5. the preparation method of a kind of disperse blue according to claim 1, it is characterised in that the water described in described step (4), hydrochloric acid, ferric chloride, disperse blue 165 coarse filtration cake mass ratio be 1～2:1:0.36～0.37:1。
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| CN201610057984.6A CN105694523A (en) | 2016-01-28 | 2016-01-28 | Preparation method of disperse blue |
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| CN201610057984.6A CN105694523A (en) | 2016-01-28 | 2016-01-28 | Preparation method of disperse blue |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115093344A (en) * | 2022-06-14 | 2022-09-23 | 绍兴市上虞金冠化工有限公司 | Preparation method of cyano-containing azo disperse dye or intermediate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4045430A (en) * | 1974-11-29 | 1977-08-30 | Bayer Aktiengesellschaft | Conversion of o-halogenoazo compound to o-cyanoazo compound by reaction with a zinc cyanide |
| CN1034215A (en) * | 1988-01-13 | 1989-07-26 | 大连工学院 | The Process for the cyanation of liquid-solid phase azoic dyestuff |
-
2016
- 2016-01-28 CN CN201610057984.6A patent/CN105694523A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4045430A (en) * | 1974-11-29 | 1977-08-30 | Bayer Aktiengesellschaft | Conversion of o-halogenoazo compound to o-cyanoazo compound by reaction with a zinc cyanide |
| CN1034215A (en) * | 1988-01-13 | 1989-07-26 | 大连工学院 | The Process for the cyanation of liquid-solid phase azoic dyestuff |
Non-Patent Citations (1)
| Title |
|---|
| 黄逊: "含氰基蓝色单偶氮分散染料及其氰化合成工艺", 《染料工业》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115093344A (en) * | 2022-06-14 | 2022-09-23 | 绍兴市上虞金冠化工有限公司 | Preparation method of cyano-containing azo disperse dye or intermediate |
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Application publication date: 20160622 |