CN101481539A - Preparation of CI 222# reactive blue - Google Patents
Preparation of CI 222# reactive blue Download PDFInfo
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Abstract
The invention provides a method for preparing CI 222# reactive blue. The method changes one-step condensation reaction conditions and acid coupling conditons, so that product transformation ratio is improved by 8%, product quality reaches requirements for qualified products, thus avoiding generating process effluent; specifically, in the method of the invention, phase transfer catalyst is added to shorten ice grinding time in the one-step condensation, therefore, reaction efficiency is greatly improved; pH value of diazo salt is adjusted to 2.0-3.5 before the acid coupling, and after alkali coupling, dye is blended to be qualified for virgin stock spray drying.
Description
Technical field
The invention belongs to active dye technical field, particularly relate to a kind of preparation method of CI 222# Reactive blue.
Background technology
Reactive dyestuffs have application performance excellence bright in colour, easy to use, distinguishing features such as suitability is strong, over nearly 20 years because the economic factors that the restriction of ecotope and the three wastes are handled and that the production of reactive dyestuffs is prepared the requirement of dye uptake, degree of fixation and dyeing waste-water is more and more higher, so the research and development of reactive dyestuffs are developed to the magma drying process with atomizing by the technology of saltouing in past, but avoid the generation of by product in the synthesis technique of magma drying process with atomizing requirement dyestuff.
The CI 222# Reactive blue molecular formula of production and selling is C on the market
37H
23ClNNa
6O
22S
7, this dyestuff no matter dye uptake, degree of fixation and other every fastness is all very good.
The synthetic method of former CI222# Reactive blue is as follows:
1) a step condensation: the adding trash ice is reduced to 0 ℃ add end water in pot after, add cyanuric chloride ice mill after 30 minutes, (the cas numbering: 2494-89-5) pH=3-5 is transferred with 10% yellow soda ash in the back to add para-ester, degree of insulation 0-5 ℃ simultaneously, reacted with this understanding 4-5 hour, and got a step condensation reaction solution.
2) two step condensations: add 2 after a step condensation is finished in a step condensation reaction solution, transfer pH=6-7 with 10% sodium carbonate solution after 4-diamino benzene sulfonic acid sodium stirs, chuck is warmed up to 40-45 ℃ simultaneously, and reacts with this understanding 2-3 hour.
3) diazotization: cool to 0 ℃ with trash ice after two step condensations are finished, add hydrochloric acid, in the 0-5 ℃ of quick Sodium Nitrite that adds, keep Sodium Nitrite excessive, promptly potassium iodide starch paper is blue, and it is blue that congo-red test paper is, and reacts to get diazotization solution in 2 hours, standby.
4) acid idol: in water, add the H acid back that stirs and transfer pH=6.5-7, the H acid solution was slowly added in the above-mentioned diazotization solution in 4-5 hour after molten entirely, finish, get sour coupling solution at 10-15 ℃ of conditioned response 8-10 hour with 10% yellow soda ash
5) alkali idol: will add in the above-mentioned sour coupling solution after the Sulpho Tobias Acid diazotization, finish the back and transfer pH=8-8.5, reacted with this understanding 2 hours, obtain final mean annual increment solution with 10% sodium carbonate solution.
6) finished productization: dyestuff is synthetic adjust to required product intensity with Sodium sulfate anhydrous.min(99) after finishing after spraying drying pack.
Above-mentioned production technique is because the quality that the acid coupling medium is lower, reaction conversion ratio is low, by product influences product so it is refining to saltout to the acid coupling thing, produces a large amount of saliferous and organic waste water like this.The new preparation method of the present invention's research and development has changed a step condensation reaction condition and a sour even condition, makes conversion rate of products improve 8%, and the generation of processing wastewater has been avoided in the requirement of the qualified product that quality product reaches.
Summary of the invention
The technical problem to be solved in the present invention is: the water-fast reaction system of cyanuric chloride is the solid-liquid two-phase reaction system in a step condensation, cyanuric chloride is difficult to complete reaction, and cyanuric chloride is met water generation hydrolytic side reactions, in the acid idol after diazotization, because medium pH＜2, H acid add reaction slowly, make that the coupling transformation efficiency is low, generate single even thing, cause that the finished product dye shade is dark, colouring is low, so the general process for purification of saltouing that adopts is removed the side reaction thing, produce waste water, the finished product dyestuff also has certain loss.The present invention provides improving one's methods of a kind of CI of preparation 222# Reactive blue for addressing the above problem, and wherein adds phase-transfer catalyst and shorten the ice time consuming in a step condensation, and reaction efficiency obviously improves like this; PH with diazonium salt before the acid idol is transferred to 2.0-3.5, and the qualified magma spraying drying of carrying out after the alkali idol is mixed dyestuff.
More specifically, the invention provides the preparation method who is prepared as follows CI 222# Reactive blue, this method comprises the steps:
A) a step condensation: add phase-transfer catalyst under the cold condition in the aqueous solution of cyanuric chloride, add para-ester after stirring, it is acid transferring pH with sodium carbonate solution, keeps 0-10 ℃ of temperature, reacts 4-5 hour, gets a step condensated liquid.
B) two step condensations: add 2 in a step condensated liquid, 4-diamino benzene sulfonic acid sodium is warmed up to 25-45 ℃ after stirring, transfer pH=4-7 with sodium carbonate solution, reacts to get two step condensated liquids in 2-3 hour.
C) diazotization: add Sodium Nitrite fast and keep Sodium Nitrite excessive after 10 ℃ of two step condensated liquids coolings are added hydrochloric acid, react and transfer pH=2.0-3.5 with sodium bicarbonate after 2 hours, get diazonium liquid.
D) the diazonium liquid that acid idol: add the H acid back that stirs and transfer pH=6.5-7 with sodium carbonate solution in water, slowly add above-mentioned c after molten entirely) step obtains reacted 8-10 hour then, sour coupling solution.
E) alkali idol: with adding in the above-mentioned sour coupling solution after the Sulpho Tobias Acid diazotization, transfer pH=8-8.5, react after 2 hours, adjust to required dye strength spraying drying with Sodium sulfate anhydrous.min(99) with sodium carbonate solution.
In this method, a) phase-transfer catalyst in the step is preferably CSC, and CSC can buy from the market.
Particularly, method of the present invention comprises following steps:
A) a step condensation: in water, add trash ice and reduce to 0 ℃, add phase-transfer catalyst CSC again after adding cyanuric chloride, stir after 10 minutes add para-ester after, transfer pH=3-5 with 10% sodium carbonate solution, keep 0-10 ℃ of temperature with trash ice simultaneously, reacted with this understanding 4-5 hour, and got a step condensated liquid.
B) two step condensations: in a step condensated liquid, add 2,4-diamino benzene sulfonic acid sodium, 30-45 ℃ of the back intensification that stir transferred pH=5-7 with 10% sodium carbonate solution simultaneously, and reacted with this understanding 2-3 hour, gets two step condensated liquids.
C) diazotization: after two steps condensated liquids adding trash ice is lowered the temperature 10 ℃, added hydrochloric acid then, add Sodium Nitrite fast, keep Sodium Nitrite excessive at 10-25 ℃, be that potassium iodide starch paper is blueness, it is blue that Congo red lion is, and reacted 2 hours, transfer pH=2.0-3.5 with sodium bicarbonate, get diazonium liquid.
D) acid is even: transfer pH=6.5-7 with 10% sodium carbonate solution after adding H acid stirs in water, complete molten back slowly added in the above-mentioned diazonium liquid in 2-5 hour and reacted 8-10 hour under 10-25 ℃ of condition, got sour coupling solution.
E) alkali idol: will add after the Sulpho Tobias Acid diazotization in the above-mentioned sour coupling solution, with 10% sodium carbonate solution accent pH=8-8.5, react 2 hours with this understanding after, adjust to required dye strength spraying drying with Sodium sulfate anhydrous.min(99).
New preparation method is by adding phase-transfer catalyst in a step condensation reaction, strengthened a step condensation reaction transformation ratio, and increased the diazotization transformation efficiency by improving the diazotization temperature, and before the acid idol, diazonium salt pH is adjusted to 2.0-3.5, thereby increased sour even reaction conditions and got a purer acidic coupling object, need not make with extra care, and then obtain quality CI 222# reactive blue dye preferably with Sulpho Tobias Acid alkali idol, method of the present invention is like this avoided purification step, thereby avoids producing waste water and dyestuff loss.The CI 222# Reactive blue that preparation method of the present invention obtains has hyperergy, good solvability and easy excellent colourability and circulation ratio such as washing and high dyefastness, be suitable for fabrics such as dyeing linen-cotton silk, have good compatibleness and degree of fixation, and directly magma spraying, no processing wastewater discharging is played promoter action to keeping environment.
Embodiment
Below by example the present invention is done detailed description, these embodiment just are used to explain technical scheme of the present invention, are not that the present invention is formed any restriction.
Particularly, the preparation method's of CI 222# reactive blue dye specific embodiment is as follows:
Embodiment 1
(1) one step condensation: in pot, add end water 200Kg, add trash ice 600Kg, add 100% cyanuric chloride 49Kg, add phase-transfer catalyst CSC0.4Kg again, stir after 10 minutes add 100% para-ester 76.87 after, transfer pH=5 in 0-5 ℃ with 10% sodium carbonate solution, and reacted with this understanding 5 hours a step condensated liquid
(2) two step condensations: 2 of back adding 100% is finished in a step condensation, 4-diamino benzene sulfonic acid sodium 55.21Kg opens chuck and heats up, and transfers pH=6-7 with 10% sodium carbonate solution simultaneously, with temperature rise to 40-45 ℃ stop heating and 40-45 ℃, pH=6-7 reaction 3 hours two step condensated liquids
(3) diazotization: after two step condensation reactions are finished, be cooled to 10 ℃ with trash ice, add 100% hydrochloric acid 22.3Kg then, add 100% Sodium Nitrite 18.5Kg then fast, keep Sodium Nitrite excessive, promptly potassium iodide starch paper is blue, it is blue that congo-red test paper is, and remained the Sodium Nitrite excessive response 2 hours at 10-20 ℃, and remove excessive nitrite sodium, transfer pH=2.0-2.2 with sodium bicarbonate, get diazonium liquid
(4) acid idol: in pot, add end water 400Kg, add 100% H acid 81.5Kg then, transfer pH=6.5-7.0 with 10% sodium carbonate solution then, the diazonium liquid that added excessive above-mentioned (3) step behind the CL in 3 hours, finish the back and under 15-20 ℃ of condition, reacted 10 hours, get sour coupling solution
(5) alkali idol: in water, add 100% Sulpho Tobias Acid 76.44Kg, add trash ice 500Kg again, add 10% Sodium Nitrite 17.77Kg fast at 0-5 ℃ after adding 100% hydrochloric acid 12.11Kg then, finishing the back keeps Sodium Nitrite excessive at 0-5 ℃, be that potassium iodide starch paper is blueness, it is blue that congo-red test paper is, reacted with this understanding 2 hours, remove excessive nitrite sodium, this diazonium liquid is joined in the above-mentioned sour coupling solution, and transfer pH=8.0-8.5, and reacted with this understanding 2 hours with 10% sodium carbonate solution, it is qualified to detect, and adjusts to required dye strength spraying drying with Sodium sulfate anhydrous.min(99).
Embodiment 2
(1) one step condensation: in pot, add end water 200Kg, add trash ice 600Kg, add 100% cyanuric chloride 49Hg, adding phase-transfer catalyst CSC 0.4Kg again stirred 10 minutes, after adding 100% para-ester 76.87 then, transfer pH=3 in 0-5 ℃ with 10% sodium carbonate solution, and reacted with this understanding 4 hours a step condensated liquid;
(2) two step condensations: add 100%2 after a step condensation is finished, 4-diamino benzene sulfonic acid sodium 55.21Kg, open chuck and heat up, simultaneously with 10% sodium carbonate solution transfer pH=6-7 with temperature rise to 30-40 ℃ stop heating and 30-40 ℃, pH=4-5 reaction 2 hours two go on foot condensated liquids;
(3) diazotization: after two step condensation reactions are finished, be cooled to 10 ℃ with trash ice, add 100% Sodium Nitrite 18.5Kg fast after adding 100% hydrochloric acid 22.3Kg, guarantor's Sodium Nitrite is excessive, be that potassium iodide starch paper is blueness, it is blue that congo-red test paper is, and remained the Sodium Nitrite excessive response 2 hours at 15-20 ℃, and remove excessive nitrite sodium, transfer pH=2.0-2.5 to get diazonium liquid with sodium bicarbonate;
(4) acid is even: add end water 400Kg in pot, add 100% H acid 81.5Kg then, transfer pH=6.5-7 with 10% sodium carbonate solution, added in the excessive diazonium liquid in 3 hours behind the CL, finish the back and reacted 9 hours under 15-20 ℃ of condition;
(5) alkali idol: in water, add 100% Sulpho Tobias Acid 76.44Kg, add trash ice 500Kg again, add 100% hydrochloric acid 12.11Kg then, add 10% Sodium Nitrite 17.77Kg fast at 0-5 ℃ then, it is excessive at 0-5 ℃ of guarantor's Sodium Nitrite to finish the back, be that potassium iodide starch paper is blueness, it is blue that congo-red test paper is, reacted with this understanding 2 hours, and removed excessive nitrite sodium, this diazonium liquid is joined in the even liquid of above-mentioned acid, transfer pH=8-8.5 with 10% sodium carbonate solution, and reacted with this understanding 1 hour, it is qualified to detect, and adjusts to required dye strength spraying drying with Sodium sulfate anhydrous.min(99).
Embodiment 3
(1) one step condensation: in pot, add end water 200Kg, add trash ice 600Kg, add 100% cyanuric chloride 49Kg, add phase-transfer catalyst CSC 0.4Kg again, stir after 10 minutes add 100% para-ester 76.87Kg after, transfer pH=3-5 in 5-10 ℃ with 10% sodium carbonate solution, and reacted with this understanding 5 hours a step condensated liquid;
(2) two step condensations: add 100%2 after a step condensation is finished, 4-diamino benzene sulfonic acid sodium 55.21Kg, open chuck and heat up, transfer pH=6-7 with 10% sodium carbonate solution simultaneously, with temperature rise to 30-35 ℃ stop heating and 30-35 ℃, pH=6-7 reaction 3 hours two go on foot condensated liquids;
(3) diazotization: after two step condensation reactions are finished, be cooled to 10 ℃ with trash ice, add 100% hydrochloric acid 22.3Kg then, add 100% Sodium Nitrite 18.5Kg then fast, guarantor's Sodium Nitrite is excessive, be that potassium iodide starch paper is blueness, it is blue that congo-red test paper is, and remained the Sodium Nitrite excessive response 2 hours at 15-20 ℃, remove excessive nitrite sodium, transfer pH=2.5-3 to get diazonium liquid with sodium bicarbonate;
(4) acid idol: in pot, add end water 400Kg, add 100% H acid 81.5Kg then, with 10% sodium carbonate solution accent pH=6.5-7, added in the excessive diazonium liquid in 2 hours behind the CL then, finish the back and under 15-20 ℃ of condition, reacted 8 hours, get sour coupling solution;
(5) alkali idol: in water, add 100% Sulpho Tobias Acid 76.44Kg, add trash ice 500Kg again, add 100% hydrochloric acid 12.11Kg, add 10% Sodium Nitrite 17.77Kg fast at 0-5 ℃ then, it is excessive at 0-5 ℃ of guarantor's Sodium Nitrite to finish the back, be that potassium iodide starch paper is blueness, it is blue that congo-red test paper is, reacted with this understanding 2 hours, remove excessive nitrite sodium, this diazonium liquid is joined in the above-mentioned sour coupling solution transfer pH=8-8.5, and reacted with this understanding 1 hour with 10% sodium carbonate solution, it is qualified to detect, and adjusts to required dye strength spraying drying with Sodium sulfate anhydrous.min(99).
Embodiment 4
(1) one step condensation: in pot, add end water 200Kg, add trash ice 600Kg, add 100% cyanuric chloride 49Kg, add phase-transfer catalyst CSC 0.4Kg again, stir after 10 minutes add 100% para-ester 76.87Kg after, transfer pH=3-5 in 5-10 ℃ with 10% sodium carbonate solution, and reacted with this understanding 4 hours, get a step condensated liquid;
(2) two step condensations: add 100%2 after a step condensation is finished, 4-diamino benzene sulfonic acid sodium 55.21Kg opens chuck and heats up, and transfers pH=6-7 with 10% sodium carbonate solution simultaneously, temperature is risen to 35-40 ℃ stops heating and 35-40 ℃, pH=6-7 reaction 3 hours, two step condensated liquids;
(3) diazotization: after two step condensation reactions are finished, be cooled to 10 ℃ with trash ice, add 100% Sodium Nitrite 18.5Kg fast after adding 100% hydrochloric acid 22.3Kg, guarantor's Sodium Nitrite is excessive, be that potassium iodide starch paper is blueness, it is blue that congo-red test paper is, and remained the Sodium Nitrite excessive response 2 hours at 20-15 ℃, remove excessive nitrite sodium and transfer pH=3.0-3.5 with sodium bicarbonate, diazonium liquid;
(4) acid idol: adding end water 400Kg in pot, add 100%H acid 81.5Kg, transfer pH=6.5-7 with 10% sodium carbonate solution, added in the excessive diazonium liquid in 2 hours behind the CL, finish the back and under 15-20 ℃ of condition, reacted 10 hours;
(5) alkali idol: in water, add 100% Sulpho Tobias Acid 76.44Kg, add trash ice 500Kg again, add 10% Sodium Nitrite 17.77Kg fast at 0-5 ℃ after adding 100% hydrochloric acid 12.11Kg, it is excessive at 0-5 ℃ of guarantor's Sodium Nitrite to finish the back, be that potassium iodide starch paper is blueness, it is blue that congo-red test paper is, reacted with this understanding 2 hours, remove excessive nitrite sodium, this diazonium liquid joined in the above-mentioned sour coupling solution with 10% sodium carbonate solution transfer pH=8-8.5 and reacted with this understanding 1 hour, it is qualified to detect, and adjusts to required dye strength spraying drying with Sodium sulfate anhydrous.min(99).
As follows by the output that the method for the foregoing description 1-4 prepares:
| Sequence number | Output | Intensity | Roll over hundred receipts amounts |
| 1 | 402 | 116 | 466.32 |
| 2 | 401 | 116 | 465.16 |
| 3 | 404 | 115 | 464.6 |
| 4 | 397 | 117 | 464.49 |
| On average | 401 | 116 | 465.16 |
Roll over hundred content=natural scale * intensity
Must measure than the old technology raising 8% of technology part after all by the product of method preparation of the present invention is actual, and this method does not have refined salt consumption and processing wastewater.
The invention discloses the novel synthesis of CI 222# Reactive blue, those skilled in the art can realize by using for reference links such as this paper content appropriate change raw material processing parameter, processing step.Method of the present invention and technology are described in detail by preferred embodiment, person skilled obviously can be waken up with a start change to methods as herein described or suitably be changed with combination and realize content of the present invention, technology in not breaking away from content spirit and scope of the present invention, special needs to be pointed out is that all similarly replace and change apparent to those skilled in the art, they will be regarded as being included in the present invention spirit range content.
Claims (4)
1, a kind of method for preparing the CI222# Reactive blue, this method comprises the steps:
(1) one step condensation: in pot, add end water 200Kg, add trash ice 600Kg, add 100% cyanuric chloride 49Kg, add phase-transfer catalyst CSC0.4Kg again, stir after 10 minutes add 100% para-ester 76.87 after, transfer pH=5 in 0-5 ℃ with 10% sodium carbonate solution, and reacted with this understanding 5 hours a step condensated liquid
(2) two step condensations: 2 of back adding 100% is finished in a step condensation, 4-diamino benzene sulfonic acid sodium 55.21Kg opens chuck and heats up, and transfers pH=6-7 with 10% sodium carbonate solution simultaneously, with temperature rise to about 40-45 ℃ stop heating and about 40-45 ℃, pH=6-7 reaction 3 hours two go on foot condensated liquids
(3) diazotization: after two step condensation reactions are finished, be cooled to 10 ℃ with trash ice, add 100% hydrochloric acid 22.3Kg then, add 100% Sodium Nitrite 18.5Kg then fast, keep Sodium Nitrite excessive, promptly potassium iodide starch paper is blue, it is blue that congo-red test paper is, and remained the Sodium Nitrite excessive response 2 hours at 10-20 ℃, and remove excessive nitrite sodium, transfer pH=2.0-2.2 with sodium bicarbonate, get diazonium liquid
(4) acid idol: in pot, add end water 400Kg, add 100% H acid 81.5Kg then, transfer pH=6.5-7 with 10% sodium carbonate solution then, the diazonium liquid that added excessive above-mentioned (3) step behind the CL in 3 hours, finish the back and under about 15-20 ℃ condition, reacted 10 hours, get sour coupling solution
(5) alkali idol: in water, add 100% Sulpho Tobias Acid 76.44Kg, add trash ice 500Kg again, add 10% Sodium Nitrite 17.77Kg fast at 0-5 ℃ after adding 100% hydrochloric acid 12.11Kg then, finishing the back keeps Sodium Nitrite excessive at 0-5 ℃, be that potassium iodide starch paper is blueness, it is blue that congo-red test paper is, reacted with this understanding 2 hours, remove excessive nitrite sodium, this diazonium liquid is joined in the above-mentioned sour coupling solution, and transfer pH=8-8.5, and reacted with this understanding 2 hours with 10% sodium carbonate solution, it is qualified to detect, and adjusts to required dye strength spraying drying with Sodium sulfate anhydrous.min(99).
2, a kind of method for preparing the CI222# Reactive blue, this method comprises the steps:
(1) one step condensation: in pot, add end water 200Kg, add trash ice 600Kg, add 100% cyanuric chloride 49Kg, adding phase-transfer catalyst CSC0.4Kg again stirred 10 minutes, after adding 100% para-ester 76.87 then, transfer pH=3 in 0-5 ℃ with 10% sodium carbonate solution, and reacted with this understanding 4 hours a step condensated liquid;
(2) two step condensations: add 100%2 after a step condensation is finished, 4-diamino benzene sulfonic acid sodium 55.21Kg, open chuck and heat up, simultaneously with 10% sodium carbonate solution transfer pH=6-7 with temperature rise to 30-40 ℃ stop heating and 30-40 ℃, pH=4-5 reaction 2 hours two go on foot condensated liquids;
(3) diazotization: after two step condensation reactions are finished, be cooled to 10 ℃ with trash ice, add 100% Sodium Nitrite 18.5Kg fast after adding 100% hydrochloric acid 22.3Kg, guarantor's Sodium Nitrite is excessive, be that potassium iodide starch paper is blueness, it is blue that congo-red test paper is, and remained the Sodium Nitrite excessive response 2 hours at 15-20 ℃, and remove excessive nitrite sodium, transfer pH=2.0-2.5 to get diazonium liquid with sodium bicarbonate;
(4) acid is even: add end water 400Kg in pot, add 100% H acid 81.5Kg then, transfer pH=6.5-7 with 10% sodium carbonate solution, added in the excessive diazonium liquid in 3 hours behind the CL, finish the back and reacted 9 hours under 15-20 ℃ of condition;
(5) alkali idol: in water, add 100% Sulpho Tobias Acid 76.44Kg, add trash ice 500Kg again, add 100% hydrochloric acid 12.11Kg then, add 10% Sodium Nitrite 17.77Kg fast at 0-5 ℃ then, it is excessive at 0-5 ℃ of guarantor's Sodium Nitrite to finish the back, be that potassium iodide starch paper is blueness, it is blue that congo-red test paper is, reacted with this understanding 2 hours, and removed excessive nitrite sodium, this diazonium liquid is joined in the even liquid of above-mentioned acid, transfer pH=8-8.5 with 10% sodium carbonate solution, and reacted with this understanding 1 hour, it is qualified to detect, and adjusts to required dye strength spraying drying with Sodium sulfate anhydrous.min(99).
3, a kind of method for preparing the CI222# Reactive blue, this method comprises the steps:
(1) one step condensation: in pot, add end water 200Kg, add trash ice 600Kg, add 100% cyanuric chloride 49Kg, add phase-transfer catalyst CSC0.4Kg again, stir after 10 minutes add 100% para-ester 76.87Kg after, transfer pH=3-5 in 5-10 ℃ with 10% sodium carbonate solution, and reacted with this understanding 5 hours a step condensated liquid;
(2) two step condensations: back adding 100% 2 is finished in a step condensation, 4-diamino benzene sulfonic acid sodium 55.21Kg, open chuck and heat up, transfer pH=6-7 with 10% sodium carbonate solution simultaneously, with temperature rise to 30-35 ℃ stop heating and 30-35 ℃, pH=6-7 reaction 3 hours two go on foot condensated liquids;
(3) diazotization: after two step condensation reactions are finished, be cooled to 10 ℃ with trash ice, add 100% hydrochloric acid 22.3Kg then, add 100% Sodium Nitrite 18.5Kg then fast, guarantor's Sodium Nitrite is excessive, be that potassium iodide starch paper is blueness, it is blue that congo-red test paper is, and remained the Sodium Nitrite excessive response 2 hours at 15-20 ℃, remove excessive nitrite sodium, transfer pH=2.5-3 to get diazonium liquid with sodium bicarbonate;
(4) acid idol: in pot, add end water 400Kg, add 100% H acid 81.5Kg then, with 10% sodium carbonate solution accent pH=6.5-7, added in the excessive diazonium liquid in 2 hours behind the CL then, finish the back and under 15-20 ℃ of condition, reacted 8 hours, get sour coupling solution;
(5) alkali idol: in water, add 100% Sulpho Tobias Acid 76.44Kg, add trash ice 500Kg again, add 100% hydrochloric acid 12.11Kg, add 10% Sodium Nitrite 17.77Kg fast at 0-5 ℃ then, it is excessive at 0-5 ℃ of guarantor's Sodium Nitrite to finish the back, be that potassium iodide starch paper is blueness, it is blue that congo-red test paper is, reacted with this understanding 2 hours, remove excessive nitrite sodium, this diazonium liquid is joined in the above-mentioned sour coupling solution transfer pH=8-8.5, and reacted with this understanding 1 hour with 10% sodium carbonate solution, it is qualified to detect, and adjusts to required dye strength spraying drying with Sodium sulfate anhydrous.min(99).
4, a kind of method for preparing the CI222# Reactive blue, this method comprises the steps:
(1) one step condensation: in pot, add end water 200Kg, add trash ice 600Kg, add 100% cyanuric chloride 49Kg, add phase-transfer catalyst CSC0.4Kg again, stir after 10 minutes add 100% para-ester 76.87Kg after, transfer pH=3-5 in 5-10 ℃ with 10% sodium carbonate solution, and reacted with this understanding 4 hours, get a step condensated liquid;
(2) two step condensations: add 100%2 after a step condensation is finished, 4-diamino benzene sulfonic acid sodium 55.21Kg opens chuck and heats up, and transfers pH=6-7 with 10% sodium carbonate solution simultaneously, temperature is risen to 35-40 ℃ stops heating and 35-40 ℃, pH=6-7 reaction 3 hours, two step condensated liquids;
(3) diazotization: after two step condensation reactions are finished, be cooled to 10 ℃ with trash ice, add 100% Sodium Nitrite 18.5Kg fast after adding 100% hydrochloric acid 22.3Kg, guarantor's Sodium Nitrite is excessive, be that potassium iodide starch paper is blueness, it is blue that congo-red test paper is, and remained the Sodium Nitrite excessive response 2 hours at 20-15 ℃, remove excessive nitrite sodium and transfer pH=3.0-3.5 with sodium bicarbonate, diazonium liquid;
(4) acid idol: adding end water 400Kg in pot, add 100%H acid 81.5Kg, transfer pH=6.5-7 with 10% sodium carbonate solution, added in the excessive diazonium liquid in 2 hours behind the CL, finish the back and under 15-20 ℃ of condition, reacted 10 hours;
(5) alkali idol: in water, add 100% Sulpho Tobias Acid 76.44Kg, add trash ice 500Kg again, add 10% Sodium Nitrite 17.77Kg fast at 0-5 ℃ after adding 100% hydrochloric acid 12.11Kg, it is excessive at 0-5 ℃ of guarantor's Sodium Nitrite to finish the back, be that potassium iodide starch paper is blueness, it is blue that congo-red test paper is, reacted with this understanding 2 hours, remove excessive nitrite sodium, this diazonium liquid joined in the above-mentioned sour coupling solution with 10% sodium carbonate solution transfer pH=8-8.5 and reacted with this understanding 1 hour, it is qualified to detect, and adjusts to required dye strength spraying drying with Sodium sulfate anhydrous.min(99).
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102796397A (en) * | 2012-08-23 | 2012-11-28 | 楚源高新科技集团股份有限公司 | Method for synthesis of active printing dye from T acid mother liquor wastewater |
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2008
- 2008-12-12 CN CNA2008101541339A patent/CN101481539A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102796397A (en) * | 2012-08-23 | 2012-11-28 | 楚源高新科技集团股份有限公司 | Method for synthesis of active printing dye from T acid mother liquor wastewater |
| CN102796397B (en) * | 2012-08-23 | 2013-07-24 | 楚源高新科技集团股份有限公司 | Method for synthesis of active printing dye from T acid mother liquor wastewater |
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Application publication date: 20090715 |