CN101633495A - Method for preparing sulphur black dye and sodium thiosulfate from sulphur dye waste water - Google Patents
Method for preparing sulphur black dye and sodium thiosulfate from sulphur dye waste water Download PDFInfo
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- CN101633495A CN101633495A CN200810022432A CN200810022432A CN101633495A CN 101633495 A CN101633495 A CN 101633495A CN 200810022432 A CN200810022432 A CN 200810022432A CN 200810022432 A CN200810022432 A CN 200810022432A CN 101633495 A CN101633495 A CN 101633495A
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Abstract
The invention relates to a method for preparing sulphur black dye and sodium thiosulfate from sulphur dye waste water, which comprises the following steps: heating sulphur dye waste water, then mixing the sulphur dye waste water with 2,4-dinitrochlorobenzol, adjusting the PH value of the mixed solution with alkali, and carrying hydrolysis reaction; mixing and stirring the sulphur dye waste water, the sodium thiosulfate and sulfur, and heating the mixture for carrying out polysulfide reaction; mixing the mixed solution of the hydrolysis reaction and the mixed solution of polysulfide reaction for sulfofication reaction, and after the reaction is finished, introducing air for oxidation reaction to obtain mixed mother solution; filtering the mixed mother solution to obtain sulphur black dye grains, and drying, grinding and blending the sulphur black dye grains to obtain commercial sulphur black dye grains; and condensing, decoloring, crystallizing, drying and screening the filtered mixed mother solution to obtain the sodium thiosulfate. The method can effectively treat sulphur dye waste water, not only solve the problem of sewage treatment, but also save large amount of clean water.
Description
Technical field
The present invention relates to producing a kind of method of chemical industry dye wastewater treatment and comprehensive utilization, specifically a kind of method of utilizing thioxine dyes waste water to prepare black sulfide dye and Sulfothiorine.
Background technology
At present, (mainly contain dyestuff intermediate and 2 in the waste water for producing the waste water that thioxine dyes produced, derivatives such as 4-sodium dinitrophenol) processing, all be basically adopt that the one-level Waste Water Treatment neutralizes, coagulation, precipitation process, the discharge of wastewater after will handling then.If handle can remove after up to standard in the waste water residual dyestuff intermediate, the COD of water outlet meets the emission request of national waste water below 100mg/l, but wastewater treatment expense per ton has increased the production cost of thioxine dyes more than 50 yuan.If production wastewater treatment does not reach the permission emission standard of national regulation and just discharged, can cause very big pollution to environment.
Summary of the invention
The object of the present invention is to provide a kind of method of utilizing thioxine dyes waste water to prepare black sulfide dye and Sulfothiorine, can effectively handle thioxine dyes waste water, available goods and materials in the waste water can be reclaimed again by this method.
For achieving the above object, the present invention adopts following scheme:
A kind of method of utilizing thioxine dyes waste water to prepare black sulfide dye and Sulfothiorine may further comprise the steps:
A) with thioxine dyes waste water heating back and 2, the 4-dinitrochlorobenzene is mixed and with behind alkali adjusting pH value to 8～9.5, the reaction that is hydrolyzed obtains the hydrolysis reaction mixed solution;
B) thioxine dyes waste water is mixed, stirs post-heating with sodium sulphite and sulphur, carry out many vulcanization reactions, obtain many vulcanization reactions mixed solution;
C) the hydrolysis reaction mixed solution is mixed, stirs, heats with many vulcanization reactions mixed solution, make them carry out vulcanization reaction, after reaction finished, bubbling air carried out oxidizing reaction again, obtains mixing mother liquor;
D) will mix mother liquor and filter, obtain the black sulfide dye particle, and again the black sulfide dye particle be carried out drying, grinding, assembly and mix, obtain the black sulfide dye finished product;
E) mother liquor after will filtering concentrate, decolouring, crystallization, oven dry and screening, obtain Sulfothiorine.
In hydrolysis reaction, thioxine dyes waste water and 2, the weight ratio between the 4-dinitrochlorobenzene are 3.5: 1～1.5: 1, and used alkali is that concentration is 20～40% sodium hydroxide or potassium hydroxide solution, the temperature of hydrolysis reaction is 50～100 ℃, and the time of reaction is 1～3 hour.
In many vulcanization reactions, the weight ratio of thioxine dyes waste water and sodium sulphite, sulfur consumption was respectively 3.5: 1～1.5: 1,3.5: 1～1.5: 1, and the temperature of many vulcanization reactions is 60～110 ℃, and the time of reaction is 3～6 hours.
The temperature of vulcanization reaction is that 100～140 ℃, pressure are that 0.15～0.25 MPa, reaction times are 6～14 hours, and the temperature of oxidizing reaction is that 60～100 ℃, time of reaction are 1～4 hour.
It is 110～140 ℃ that the black sulfide dye particle is carried out the exsiccant temperature, be 4～8 hours time of drying, drying efficiency is 80～120kg/h, milling time is 4～6 hours, black sulfide dye particle after the grinding can be crossed 80 mesh sieves more than 95%, piecing together the stirring velocity of mixing is 20～80 rev/mins, and churning time is 6～8 hours.
Mixing mother liquor after the filtration concentrates, existing Sulfothiorine vacuum multi-effect evaporation system is adopted in decolouring, crystallization, oven dry, and its whole technological process is same as the prior art.
The present invention can effectively handle thioxine dyes waste water, has promptly solved the problem of sewage disposal, a large amount of clean water that can save again.To produce 10000 tons of black sulfide dyes per year is example, but 15628 tons/year of water saving, reduce discharging 17460 tons/year in sewage, reduce 1.12 tons/year of COD quantity dischargeds, reduce 0.208 ton/year of ammonia nitrogen quantity discharged, save 87.3 ten thousand yuan of plant effuent handlings, both alleviated the quantity discharged of existing plant effuent, realize the comprehensive regulation of sewage again, reached the purpose of energy-saving and emission-reduction, cleaner production.
Embodiment
Further specify the present invention below in conjunction with embodiment.
Embodiment 1
1, thioxine dyes waste water 250KG is added in the reactor 1, after being heated to 60 ℃, under the state that stirs, add 2,4-dinitrochlorobenzene 100KG, after the sodium hydroxide solution of adding 30% is regulated pH value to 8 in mixing process, the reaction that is hydrolyzed, the reaction times is 1.5 hours, obtains the hydrolysis reaction mixed solution;
2, thioxine dyes waste water 250KG is added in the reactor 2, add sodium sulphite and the sulphur of each 100KG respectively under the state that stirs, be heated to 70 ℃, carry out many vulcanization reactions, the reaction times is 4 hours, obtains many vulcanization reactions mixed solution;
3, the many vulcanization reactions mixed solution in the reactor 2 is joined in the reactor 1 mix with the hydrolysis reaction mixed solution, under the state that stirs, carry out vulcanization reaction, 110 ℃ of temperature of reaction, pressure 0.15 MPa, 12 hours time is after reaction finishes, carry out oxidizing reaction to reactor 1 bubbling air, 70 ℃ of oxidizing reaction temperatures, oxidation time 2 hours obtains mixing mother liquor;
4, will mix mother liquor and squeeze into strainer with pump, and adopt the rotary flash distillation mode to carry out drying treatment to the solid product that obtains after filtering, drying temperature is 120 ℃, and be 5 hours time of drying, and drying efficiency is 90kg/h; Dried solid product ground earlier 4 hours, and what make solid product after the grinding can pass through 80 mesh sieves more than 95%, pieced together mixedly then, and the stirring velocity of piecing together when mixing is 40 rev/mins, and churning time is 6 hours, obtains the black sulfide dye finished product;
5, the mother liquor that filters out enters the vacuum multi-effect evaporation system of Sulfothiorine, the vacuum multi-effect evaporation system is an existing installation, 60 ℃ of temperature, under pressure-0.1 MPa, same as the prior art concentrate by adopting, decolouring, crystallization, oven dry and screening operation, obtain the Sulfothiorine finished product.
Embodiment 2
1, thioxine dyes waste water 300KG is added in the reactor 1, after being heated to 80 ℃, under the state that stirs, add 2,4-dinitrochlorobenzene 100KG, after the sodium hydroxide solution of adding 30% is regulated pH value to 9 in mixing process, the reaction that is hydrolyzed, the reaction times is 2 hours, obtains the hydrolysis reaction mixed solution;
2, thioxine dyes waste water 350KG is added in the reactor 2, add sodium sulphite and the sulphur of each 150KG respectively under the state that stirs, be heated to 90 ℃, carry out many vulcanization reactions, the reaction times is 5 hours, obtains many vulcanization reactions mixed solution;
3, the many vulcanization reactions mixed solution in the reactor 2 is joined in the reactor 1 mix with the hydrolysis reaction mixed solution, under the state that stirs, carry out vulcanization reaction, 120 ℃ of temperature of reaction, pressure 0.2 MPa, 10 hours time is after reaction finishes, carry out oxidizing reaction to reactor 1 bubbling air, 85 ℃ of oxidizing reaction temperatures, oxidation time 3 hours obtains mixing mother liquor;
4, will mix mother liquor and squeeze into strainer with pump, and adopt the rotary flash distillation mode to carry out drying treatment to the solid product that obtains after filtering, drying temperature is 130 ℃, and be 6 hours time of drying, and drying efficiency is 100kg/h; Dried solid product ground earlier 5 hours, and what make solid product after the grinding can pass through 80 mesh sieves more than 95%, pieced together mixedly then, and the stirring velocity of piecing together when mixing is 60 rev/mins, and churning time is 7 hours, obtains the black sulfide dye finished product;
5, the mother liquor that filters out enters the vacuum multi-effect evaporation system of Sulfothiorine, the vacuum multi-effect evaporation system is an existing installation, 80 ℃ of temperature, under pressure-0.1 MPa, same as the prior art concentrate by adopting, decolouring, crystallization, oven dry and screening operation, obtain the Sulfothiorine finished product.
Embodiment 3
1, thioxine dyes waste water 400KG is added in the reactor 1, after being heated to 100 ℃, under the state that stirs, add 2,4-dinitrochlorobenzene 200KG, after the potassium hydroxide solution of adding 30% is regulated pH value to 9.5 in mixing process, the reaction that is hydrolyzed, the reaction times is 3 hours, obtains the hydrolysis reaction mixed solution;
2, thioxine dyes waste water 400KG is added in the reactor 2, add sodium sulphite and the sulphur of each 200KG respectively under the state that stirs, be heated to 100 ℃, carry out many vulcanization reactions, the reaction times is 6 hours, obtains many vulcanization reactions mixed solution;
3, the many vulcanization reactions mixed solution in the reactor 2 is joined in the reactor 1 mix with the hydrolysis reaction mixed solution, under the state that stirs, carry out vulcanization reaction, 130 ℃ of temperature of reaction, pressure 0.25 MPa, 8 hours time is after reaction finishes, carry out oxidizing reaction to reactor 1 bubbling air, 95 ℃ of oxidizing reaction temperatures, oxidation time 4 hours obtains mixing mother liquor;
4, will mix mother liquor and squeeze into strainer with pump, and adopt the rotary flash distillation mode to carry out drying treatment to the solid product after filtering, drying temperature is 140 ℃, and be 7 hours time of drying, and drying efficiency is 110kg/h; Dried solid product ground earlier 6 hours, and what make solid product after the grinding can pass through 80 mesh sieves more than 95%, pieced together mixedly then, and the stirring velocity of piecing together when mixing is 70 rev/mins, and churning time is 8 hours, obtains the black sulfide dye finished product;
5, the mother liquor that filters out enters the vacuum multi-effect evaporation system of Sulfothiorine, the vacuum multi-effect evaporation system is an existing installation, 80 ℃ of temperature, under pressure-0.1 MPa, same as the prior art concentrate by adopting, decolouring, crystallization, oven dry and screening operation, obtain the Sulfothiorine finished product.
More than the physical and chemical index of the black sulfide dye that obtains of each embodiment as follows: granularity 80 mesh sieves can be by more than 95%, intensity 100%, coloured light: approximate, dispersion grade; The physical and chemical index of the Sulfothiorine that obtains is as follows: content: 〉=99%, and water-insoluble impurity :≤0.01%.
Claims (5)
1, a kind of method of utilizing thioxine dyes waste water to prepare black sulfide dye and Sulfothiorine is characterized in that may further comprise the steps:
A) with thioxine dyes waste water heating back and 2, the 4-dinitrochlorobenzene is mixed and with behind alkali adjusting pH value to 8～9.5, the reaction that is hydrolyzed obtains the hydrolysis reaction mixed solution;
B) thioxine dyes waste water is mixed, stirs post-heating with sodium sulphite and sulphur, carry out many vulcanization reactions, obtain many vulcanization reactions mixed solution;
C) the hydrolysis reaction mixed solution is mixed, stirs, heats with many vulcanization reactions mixed solution, make them carry out vulcanization reaction, after reaction finished, logical again people's air carried out oxidizing reaction, obtains mixing mother liquor;
D) will mix mother liquor and filter, obtain the black sulfide dye particle, and again the black sulfide dye particle be carried out drying, grinding, assembly and mix, obtain the black sulfide dye finished product;
E) the mixing mother liquor after will filtering concentrate, decolouring, crystallization, oven dry and screening, obtain Sulfothiorine.
2, the method for utilizing thioxine dyes waste water to prepare black sulfide dye and Sulfothiorine according to claim 1, it is characterized in that: thioxine dyes waste water and 2, the weight ratio of the consumption between the 4-dinitrochlorobenzene is 3.5: 1～1.5: 1, used alkali is that concentration is 20～40% sodium hydroxide or potassium hydroxide solution, the temperature of hydrolysis reaction is 50～100 ℃, and the time of reaction is 1～3 hour.
3, the method for utilizing thioxine dyes waste water to prepare black sulfide dye and Sulfothiorine according to claim 1, it is characterized in that: the weight ratio of thioxine dyes waste water and sodium sulphite, sulfur consumption is for being respectively 3.5: 1～1.5: 1,3.5: 1～1.5: 1, the temperature of many vulcanization reactions is 60～110 ℃, and the time of reaction is 3～6 hours.
4, the method for utilizing thioxine dyes waste water to prepare black sulfide dye and Sulfothiorine according to claim 1, it is characterized in that: the temperature of vulcanization reaction is that 100～140 ℃, pressure are that 0.15～0.25 MPa, reaction times are 6～14 hours, and the temperature of oxidizing reaction is that 60～100 ℃, time of reaction are 1～4 hour.
5, the method for utilizing thioxine dyes waste water to prepare black sulfide dye and Sulfothiorine according to claim 1, it is characterized in that: it is 110～140 ℃ that the black sulfide dye particle is carried out the exsiccant temperature, be 4～8 hours time of drying, drying efficiency is 80～120kg/h, milling time is 4～6 hours, black sulfide dye particle after the grinding can be crossed 80 mesh sieves more than 95%, and piecing together the stirring velocity of mixing is 20～80 rev/mins, and churning time is 6～8 hours.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992469A (en) * | 2012-12-07 | 2013-03-27 | 山东汇海医药化工有限公司 | Method for treating sodium sulfide waste water |
| CN104609618A (en) * | 2015-01-21 | 2015-05-13 | 绍兴奇彩化工有限公司 | Method for treating disperse blue 56 reducing mother-liquor wastewater |
| CN106242186A (en) * | 2016-08-31 | 2016-12-21 | 浙江奇彩环境科技股份有限公司 | A kind of recycling processing method of sulphur black technique waste water |
| CN113582849A (en) * | 2020-04-30 | 2021-11-02 | 浙江省常山长盛化工有限公司 | Method for producing sulfur black based on mixed low oil of physically purified 2, 4-dinitrochlorobenzene |
| CN115893695A (en) * | 2021-09-29 | 2023-04-04 | 中国石油化工股份有限公司 | Method for producing sodium thiosulfate by utilizing catalytic cracking flue gas desulfurization wastewater |
| CN115893695B (en) * | 2021-09-29 | 2024-07-02 | 中国石油化工股份有限公司 | Method for producing sodium thiosulfate by using catalytic cracking flue gas desulfurization wastewater |
-
2008
- 2008-07-21 CN CN200810022432A patent/CN101633495A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992469A (en) * | 2012-12-07 | 2013-03-27 | 山东汇海医药化工有限公司 | Method for treating sodium sulfide waste water |
| CN104609618A (en) * | 2015-01-21 | 2015-05-13 | 绍兴奇彩化工有限公司 | Method for treating disperse blue 56 reducing mother-liquor wastewater |
| CN106242186A (en) * | 2016-08-31 | 2016-12-21 | 浙江奇彩环境科技股份有限公司 | A kind of recycling processing method of sulphur black technique waste water |
| CN106242186B (en) * | 2016-08-31 | 2019-04-30 | 浙江奇彩环境科技股份有限公司 | A kind of recycling processing method of sulphur black technique waste water |
| CN113582849A (en) * | 2020-04-30 | 2021-11-02 | 浙江省常山长盛化工有限公司 | Method for producing sulfur black based on mixed low oil of physically purified 2, 4-dinitrochlorobenzene |
| CN115893695A (en) * | 2021-09-29 | 2023-04-04 | 中国石油化工股份有限公司 | Method for producing sodium thiosulfate by utilizing catalytic cracking flue gas desulfurization wastewater |
| CN115893695B (en) * | 2021-09-29 | 2024-07-02 | 中国石油化工股份有限公司 | Method for producing sodium thiosulfate by using catalytic cracking flue gas desulfurization wastewater |
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Open date: 20100127 |