CN102796397B - Method for synthesis of active printing dye from T acid mother liquor wastewater - Google Patents
Method for synthesis of active printing dye from T acid mother liquor wastewater Download PDFInfo
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Abstract
The invention relates to a method for synthesis of an active printing dye from T acid mother liquor wastewater and belongs to the technical field of chemical engineering. The method realizes synthesis of the active printing dye by condensation, diazotization and coupling elementary reactions. The active printing dye obtained by the method has high dissolvability, low substantivity, strong lifting power, high quality and a low production cost, can completely satisfy quality and cost requirements from printing and dyeing customers, has a high market promotion value, and further promotes sustainable production of an H acid. The method effectively reduces organic components of T acid mother liquor wastewater and is convenient for standardized discharge of T acid mother liquor wastewater.
Description
Technical field
The present invention relates to a kind of method of the T of utilization acid mother liquor waste water composite reactive thickening agent, belong to chemical technology field.
Background technology
H acid is a kind of special-purpose intermediate of making dyestuff, is widely used in industries such as printing and dyeing, weaving, chemical industry.Traditional H acid production process when obtaining target product H acid, produces a large amount of waste water, and is wherein maximum and the most difficult with T acid mother liquor waste water proportion.T acid mother liquor waste water mainly is that organism is without recovery through qualified discharge after the waste water comprehensive treating process at present, and its effective value is unrealized.Thus the influence that brings of problem severe inhibition the normal development of H acid industry.
T acid mother liquor waste water is as the waste water of H acid production process maximum, its important component is 3.5.7-trisulfonic acid naphthylamines and 4.6.8-trisulfonic acid naphthylamines and a large amount of inorganic salt ammonium sulfate etc., the COD(oxygen-consumption) content 70,000 mg/l, inorganic salt content 400,000 mg/l, at present, the T acid mother liquor waste water treatment process of none economical rationality still at home and abroad.The structural performance that contains amino and multi-sulfonic in view of organism in the T acid mother liquor, adopt friendly process with after wherein organism reclaims, make it as dyestuff intermediate, direction to the composite reactive thickening agent is researched and developed, and make with this synthetic reactive printing dyes and have higher solvability and lower substantivity, be the task that we need to be resolved hurrily.
Summary of the invention
The objective of the invention is to: a kind of T acid mother liquor waste water that rationally utilizes is provided, it is turned waste into wealth, and effectively reduce organic composition in the T acid mother liquor waste water, be convenient to the method for utilizing T acid mother liquor waste water reclamation thing composite reactive thickening agent of T acid mother liquor discharged wastewater met the national standard.
Technical scheme of the present invention is:
A kind of method of utilizing T acid mother liquor waste water composite reactive thickening agent, it is characterized in that: it may further comprise the steps:
1), the pre-treatment of T acid mother liquor water:
T acid mother liquor waste water and tertiary butyl quaternary ammonium salt are pressed 4:1 ~ 6:1 mixed, start to stir simultaneously, stirring velocity is 100 ~ 120rpm, mix 30 minutes after, leave standstill layering in 1 hour, the gained water reclaims by product ammonium sulfate by conventional concentration technology; The gained organic phase adds liquid caustic soda adjusting organic phase pH=6.0 ~ 6.5 and carries out back extraction, the gained strip liquor is by the common process concentrating under reduced pressure, it is qualified reaching 110 ~ 140g/kg until amino value wherein, and obtaining 3.5.7-trisulfonic acid naphthylamines and 4.6.8-trisulfonic acid naphthylamines is the T pickling agent of major ingredient;
2), one contracts:
Para-ester dry powder is added entry, add sodium bicarbonate simultaneously, so that para-ester dissolves fully, control PH is 6.5-7.0, afterwards it is added in 1.0 hours the cyanuric chloride of making beating ice mill, the joining day is controlled at and added in 1 hour, is that to transfer PH be 2.5-3.0 for 15% sodium bicarbonate with quality, 5-8 ℃ of system temperatures keep this pH value 2.5-3.0,5-8 ℃ of reactions of temperature 4 hours; Detect the colourless terminal point that is with amino reagent;
3), two contract:
With 2,4-diamino benzene sulfonic acid dry powder is added to one in the step 2 and contracts in the thing, and transferring PH with sodium bicarbonate is 3.5-4.0, and in 1 hour, be warming up to 35 ℃, keep this pH value 3.5-4.0,35 ℃ of reactions of temperature 5 hours, detect 2 with chromatogram, the 4-diamino benzene sulfonic acid is terminal point less than 0.3%;
4), diazonium:
Above-mentioned two things that contract are cooled to 10 ℃, transferring PH with sodium carbonate solution is 8.0-8.5, add Sodium Nitrite again, stir after 0.5 hour, in 0.5-1.5 hours, two contract inferior sodium mixtures are dripped and enter in the mixture of HCL and frozen water, reinforced process temperature is controlled at 8-10 ℃, and reaction mass remains potassiumiodide, congo-red test paper are blue, keeps after 3 hours to add sulfanilamide (SN) with cancellation nitrous acid.
5) a, coupling:
Add entry at H acid dry powder, add the liquid caustic soda dissolving simultaneously and transfer PH to 6.5-7.0, during in temperature＜10 ℃, it was dropped in 1.5-2.5 hour in the diazonium salt of step 4, transfer pH value to 3.0 with sodium bicarbonate again, 5-8 ℃ of temperature, keep under PH=3.0-3.5 condition moistening the circle method to saltout after 10 hours, detect the diazonium salt disappearance and be terminal point.
6), secondary diazonium:
Add frozen water and HCL in the T pickling agent, add Sodium Nitrite afterwards, added in 2.0 hours, reinforced process temperature is controlled at 5-8 ℃, and reaction mass remains potassiumiodide, congo-red test paper are blue, adds sulfanilamide (SN) cancellation nitrous acid after 2 hours.
7), secondary coupling:
In conjugates of secondary diazonium thing adding with step 6, transfer PH to 7.0-8.0 with yellow soda ash, 5-8 ℃ of temperature, keep under the PH=8.0 condition after 8 hours, material is by red stain indigo plant, with the profit circle method of saltouing, detect the diazonium salt disappearance and be terminal point, get reactive printing dyes.
Beneficial effect of the present invention is:
Adopt synthetic reactive printing dyes of the present invention, have higher solvability and lower substantivity, and lifting force is good, the lower characteristics of higher quality and production cost are arranged, can satisfy vast printing and dyeing client's quality and cost requirement fully, have higher market popularization value, further promote the Sustainable Production of H acid, originally effectively reduce simultaneously the organic composition in the T acid mother liquor waste water, be convenient to T acid mother liquor standard wastewater discharge.
Embodiment
Embodiment 1:
1), the pre-treatment of T acid mother liquor water:
T acid mother liquor waste water and tertiary butyl quaternary ammonium salt are pressed the 4:1 mixed, start to stir simultaneously, stirring velocity is 100rpm, mix 30 minutes after, leave standstill layering in 1 hour, the gained water reclaims by product ammonium sulfate by conventional concentration technology; The gained organic phase adds liquid caustic soda adjusting organic phase pH=6.0 and carries out back extraction, the gained strip liquor is by the common process concentrating under reduced pressure, it is qualified reaching 110g/kg until amino value wherein, and obtaining 3.5.7-trisulfonic acid naphthylamines and 4.6.8-trisulfonic acid naphthylamines is the T pickling agent of major ingredient;
2), one contracts:
The para-ester dry powder of 126.5kg is added to 450L water, add the 90kg sodium bicarbonate powder simultaneously so that para-ester dissolves clarification fully, regulating PH is 6.5, be added to afterwards in 1.0 hours the 84kg cyanuric chloride of ice mill of having pulled an oar, add in 1 hour, with quality be 15% sodium bicarbonate to transfer PH be 2.5,7 ℃ of system temperatures, keep this pH value 2.5,7 ℃ of reactions of temperature 4 hours, detect the colourless terminal point that is with amino reagent.
3), two contract:
With 2 of 75.6kg, 4-diamino benzene sulfonic acid dry powder is added to one in the step 2 and contracts in the thing, and transferring PH with sodium bicarbonate is 3.5, and in 1 hour, be warming up to 35 ℃, keep this pH value 3.5,35 ℃ of reactions of temperature 5 hours, detect 2 with chromatogram, the 4-diamino benzene sulfonic acid is terminal point less than 0.3%.
4), diazonium:
Above-mentioned two things that contract are cooled to 10 ℃, transferring PH with sodium carbonate solution is 8.0, add Sodium Nitrite 32.9kg again, stir after 0.5 hour, at 0.5 hour two contract inferior sodium mixtures are dripped and enter in the mixture of 41kgHCL and 900Kg frozen water, reinforced process temperature is controlled at 8 ℃, and reaction mass remains potassiumiodide, congo-red test paper are blue, keeps after 3 hours to add sulfanilamide (SN) with cancellation nitrous acid.
5) a, coupling:
In the H of 145.8kg acid dry powder, add water 675L, while liquid feeding alkali dissolution is also transferred PH to 6.5, during in temperature＜10 ℃, this material was dropped in 1.5 hours in the diazonium salt of step 4, transfer PH to 3.0 with sodium bicarbonate again, 7 ℃ of temperature, keep under the PH=3.0 condition moistening the circle method to saltout after 10 hours, detect the diazonium salt disappearance and be terminal point.
6), secondary diazonium:
At the 172.2kgT pickling agent with frozen water 675L, HCL33kg, add Sodium Nitrite 32.5kg afterwards, add in 2.0 hours, reinforced process temperature is controlled at 6 ℃, reaction mass remains potassiumiodide, congo-red test paper is blue, adds sulfanilamide (SN) cancellation nitrous acid after 2 hours.
7), secondary coupling:
In conjugates of secondary diazonium thing adding with step 6, transfer PH to 8.0 with yellow soda ash, 8 ℃ of temperature, keep under the PH=8.0 condition after 8 hours, material is by red stain indigo plant, with the profit circle method of saltouing, detect the diazonium salt disappearance and be terminal point, get the Reactive blue-M3G of reactive printing dyes.
Embodiment 2:
1), the pre-treatment of T acid mother liquor water:
T acid mother liquor waste water and tertiary butyl quaternary ammonium salt are pressed the 5:1 mixed, start to stir simultaneously, stirring velocity is 120rpm, mix 30 minutes after, leave standstill layering in 1 hour, the gained water reclaims by product ammonium sulfate by conventional concentration technology; The gained organic phase adds liquid caustic soda adjusting organic phase pH=6.5 and carries out back extraction, the gained strip liquor is by the common process concentrating under reduced pressure, it is qualified reaching 120g/kg until amino value wherein, and obtaining 3.5.7-trisulfonic acid naphthylamines and 4.6.8-trisulfonic acid naphthylamines is the T pickling agent of major ingredient;
2), one contracts:
The para-ester dry powder of 189.8kg is added to 675L water, add 135 kilograms of sodium bicarbonate powders simultaneously so that para-ester dissolves clarification fully, regulating PH is 6.8, be added to afterwards in 1.0 hours the 126kg cyanuric chloride of ice mill of having pulled an oar, 1.0 add in hour, with quality be 15% sodium bicarbonate to transfer PH be 3.0,6 ℃ of system temperatures, keep this pH value 3.0,6 ℃ of reactions of temperature 4 hours, detect the colourless terminal point that is with amino reagent.
3), two contract:
With 2 of 113.4kg, 4-diamino benzene sulfonic acid dry powder is added to one in the step 2 and contracts in the thing, and transferring PH with sodium bicarbonate is 3.8, and in 1 hour, be warming up to 35 ℃, keep this pH value 3.8,35 ℃ of reactions of temperature 5 hours, detect 2 with chromatogram, the 4-diamino benzene sulfonic acid is terminal point less than 0.3%.
4), diazonium:
Above-mentioned two things that contract are cooled to 10 ℃, transferring PH with sodium carbonate solution is 8.3, add Sodium Nitrite 49.35kg again, stir after 0.5 hour, at 1 hour two contract inferior sodium mixtures are dripped and enter in the mixture of 61.5kgHCL and 1350Kg frozen water, reinforced process temperature is controlled at 9 ℃, and reaction mass remains potassiumiodide, congo-red test paper are blue, keeps after 3 hours to add sulfanilamide (SN) with cancellation nitrous acid.
5) a, coupling:
In the H of 218.7kg acid dry powder, add water 1012.5L, while liquid feeding alkali dissolution is also transferred PH to 6.8, during in temperature＜10 ℃, this material was dropped in 2.0 hours in the diazonium salt of step 4, transfer PH to 3.0 with sodium bicarbonate again, 8 ℃ of temperature, keep under the PH=3.0 condition moistening the circle method to saltout after 10 hours, detect the diazonium salt disappearance and be terminal point.
6), secondary diazonium:
At the 258.3kgT pickling agent with frozen water 1012.2L, HCL49.5kg, add Sodium Nitrite 48.7kg afterwards, add in 2.0 hours, reinforced process temperature is controlled at 7 ℃, reaction mass remains potassiumiodide, congo-red test paper is blue, adds sulfanilamide (SN) cancellation nitrous acid after 2 hours.
7), secondary coupling:
In conjugates of secondary diazonium thing adding with step 6, transfer PH to 8.0 with yellow soda ash, 8 ℃ of temperature, keep under the PH=8.0 condition after 8 hours, material is by red stain indigo plant, with the profit circle method of saltouing, detect the diazonium salt disappearance and be terminal point, get the Reactive blue-M3G of reactive printing dyes.
Embodiment 3:
1), the pre-treatment of T acid mother liquor water:
T acid mother liquor waste water and tertiary butyl quaternary ammonium salt are pressed the 6:1 mixed, start to stir simultaneously, stirring velocity is 120rpm, mix 30 minutes after, leave standstill layering in 1 hour, the gained water reclaims by product ammonium sulfate by conventional concentration technology; The gained organic phase adds liquid caustic soda adjusting organic phase pH=6.5 and carries out back extraction, the gained strip liquor is by the common process concentrating under reduced pressure, it is qualified reaching 140g/kg until amino value wherein, and obtaining 3.5.7-trisulfonic acid naphthylamines and 4.6.8-trisulfonic acid naphthylamines is the T pickling agent of major ingredient;
2), one contracts:
The para-ester dry powder of 284.7kg is added to 1013L water, add sodium bicarbonate powder 203kg simultaneously so that para-ester dissolves clarification fully, regulating PH is 7.0, be added to afterwards in 1.0 hours the 189kg cyanuric chloride of ice mill of having pulled an oar, add in 1 hour, with quality be 15% sodium bicarbonate to transfer PH be 2.8,8 ℃ of system temperatures, keep this pH value 2.8,8 ℃ of reactions of temperature 4 hours, detect the colourless terminal point that is with amino reagent.
3), two contract:
With 2 of 170.1kg, 4-diamino benzene sulfonic acid dry powder is added to one in the step 2 and contracts in the thing, and transferring PH with sodium bicarbonate is 4.0, and in 1 hour, be warming up to 35 ℃, keep this pH value 4.0,35 ℃ of reactions of temperature 5 hours, detect 2 with chromatogram, the 4-diamino benzene sulfonic acid is terminal point less than 0.3%.
4), diazonium:
Above-mentioned two things that contract are cooled to 10 ℃, transferring PH with sodium carbonate solution is 8.5, add Sodium Nitrite 74.0kg again, stir after 0.5 hour, in 1.5 hours, two contract inferior sodium mixtures are dripped and enter in the mixture of 92.3kgHCL and 2025kg frozen water, reinforced process temperature is controlled at 10 ℃, and reaction mass remains potassiumiodide, congo-red test paper are blue, keeps after 3 hours to add sulfanilamide (SN) with cancellation nitrous acid.
5) a, coupling:
In the H of 328.1kg acid dry powder, add water 1518.8L, while liquid feeding alkali dissolution is also transferred PH to 7.0, during in temperature＜10 ℃ this material was dropped in 2.5 hours in the diazonium salt of step 4, transfer PH to 3.0 with sodium bicarbonate again, 9 ℃ of temperature, keep under the PH=3.0 condition moistening the circle method to saltout after 10 hours, detect the diazonium salt disappearance and be terminal point.
6), secondary diazonium:
At the 387.5kgT pickling agent with frozen water 1518.8L, 74kgHCL, add Sodium Nitrite 73.1kg afterwards, add in 2.0 hours, reinforced process temperature is controlled at 8 ℃, reaction mass remains potassiumiodide, congo-red test paper is blue, adds sulfanilamide (SN) cancellation nitrous acid after 2 hours.
7), secondary coupling:
In conjugates of secondary diazonium thing adding with step 6, transfer PH to 8.0 with yellow soda ash, 8 ℃ of temperature, keep under the PH=8.0 condition after 8 hours, material is by red stain indigo plant, with the profit circle method of saltouing, detect the diazonium salt disappearance and be terminal point, get the Reactive blue-M3G of reactive printing dyes.
Claims (1)
1. method of utilizing T acid mother liquor waste water composite reactive thickening agent, it is characterized in that: it may further comprise the steps:
1), the pre-treatment of T acid mother liquor water:
T acid mother liquor waste water and tertiary butyl quaternary ammonium salt are pressed 4:1 ~ 6:1 mixed, start to stir simultaneously, stirring velocity is 100 ~ 120rpm, mix 30 minutes after, leave standstill layering in 1 hour, the gained water reclaims by product ammonium sulfate by conventional concentration technology; The gained organic phase adds liquid caustic soda adjusting organic phase pH=6.0 ~ 6.5 and carries out back extraction, the gained strip liquor is by the common process concentrating under reduced pressure, it is qualified reaching 110 ~ 140g/kg until amino value wherein, and obtaining 3.5.7-trisulfonic acid naphthylamines and 4.6.8-trisulfonic acid naphthylamines is the T pickling agent of major ingredient;
2), one contracts:
Para-ester dry powder is added entry, add sodium bicarbonate simultaneously, so that para-ester dissolves fully, control PH is 6.5-7.0, afterwards it is added in 1.0 hours the cyanuric chloride of making beating ice mill, the joining day is controlled at and added in 1 hour, is that to transfer PH be 2.5-3.0 for 15% sodium bicarbonate with quality, 5-8 ℃ of system temperatures keep this pH value 2.5-3.0,5-8 ℃ of reactions of temperature 4 hours; Detect the colourless terminal point that is with amino reagent;
3), two contract:
With 2,4-diamino benzene sulfonic acid dry powder is added to one in the step 2 and contracts in the thing, and transferring PH with sodium bicarbonate is 3.5-4.0, and in 1 hour, be warming up to 35 ℃, keep this pH value 3.5-4.0,35 ℃ of reactions of temperature 5 hours, detect 2 with chromatogram, the 4-diamino benzene sulfonic acid is terminal point less than 0.3%;
4), diazonium:
Above-mentioned two things that contract are cooled to 10 ℃, transferring PH with sodium carbonate solution is 8.0-8.5, add Sodium Nitrite again, stir after 0.5 hour, in 0.5-1.5 hours, two contract inferior sodium mixtures are dripped and enter in the mixture of HCL and frozen water, reinforced process temperature is controlled at 8-10 ℃, and reaction mass remains potassiumiodide, congo-red test paper are blue, keeps after 3 hours to add sulfanilamide (SN) with cancellation nitrous acid;
5) a, coupling:
Add entry at H acid dry powder, add the liquid caustic soda dissolving simultaneously and transfer PH to 6.5-7.0, during in temperature＜10 ℃, it was dropped in 1.5-2.5 hour in the diazonium salt of step 4, transfer pH value to 3.0 with sodium bicarbonate again, 5-8 ℃ of temperature, keep under PH=3.0-3.5 condition moistening the circle method to saltout after 10 hours, detect the diazonium salt disappearance and be terminal point;
6), secondary diazonium:
Add frozen water and HCL in the T pickling agent, add Sodium Nitrite afterwards, added in 2.0 hours, reinforced process temperature is controlled at 5-8 ℃, and reaction mass remains potassiumiodide, congo-red test paper are blue, adds sulfanilamide (SN) cancellation nitrous acid after 2 hours;
7), secondary coupling:
In conjugates of secondary diazonium thing adding with step 6, transfer PH to 7.0-8.0 with yellow soda ash, 5-8 ℃ of temperature, keep under the PH=8.0 condition after 8 hours, material is by red stain indigo plant, with the profit circle method of saltouing, detect the diazonium salt disappearance and be terminal point, get reactive printing dyes.
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| CN106590012B (en) * | 2016-11-30 | 2019-03-12 | 浙江秦燕科技股份有限公司 | The isomer mixture of CLT acid prepares the method and product of acid dyes original powder |
| CN106590013B (en) * | 2016-11-30 | 2019-03-05 | 浙江秦燕科技股份有限公司 | The isomer mixture of CLT acid prepares acid dyes original powder and product |
| CN116285410A (en) * | 2023-02-09 | 2023-06-23 | 内蒙古新亚化工有限公司 | Integrated preparation method of double-medium acid peach red |
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