CN105233658A - Sulfur-containing wastewater comprehensive utilization method and application thereof to nicosulfuron production - Google Patents

Sulfur-containing wastewater comprehensive utilization method and application thereof to nicosulfuron production Download PDF

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CN105233658A
CN105233658A CN201510770088.XA CN201510770088A CN105233658A CN 105233658 A CN105233658 A CN 105233658A CN 201510770088 A CN201510770088 A CN 201510770088A CN 105233658 A CN105233658 A CN 105233658A
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sulfur
comprehensive utilization
solution
waste water
tail gas
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CN105233658B (en
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王春
王多余
张坤峰
顾成旺
刘改玲
蔡冲
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ANHUI KELIHUA CHEMICAL CO LTD
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ANHUI KELIHUA CHEMICAL CO LTD
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Abstract

The invention discloses a sulfur-containing wastewater comprehensive utilization method and application thereof to nicosulfuron production. The comprehensive utilization method includes the steps that tail gas containing HCl and SO2 is absorbed through two-stage falling films to generate a Na2SO3 solution for use; the Na2SO3 solution reacts with acid to generate SO2, the generated SO2 reacts with tail gas containing H2S to generate simple substance S, sulfur is obtained after filtering, and filter liquor is further oxidized into Na2SO4; excess SO2 is absorbed by alkali liquor and then enters the two-stage falling films for the HCl and SO2tail gas to be absorbed for use. The comprehensive utilization method is suitable for industrial production, the treatment effect on sulfur-containing wastewater is good, secondary pollution like dangerous solid waste is avoided, wastewater treatment is low in cost, the operation process is easy and convenient, the equipment investment is low, the recovered sulfur can be recycled, and the targets of waste control by waste and recycling economy are achieved.

Description

A kind of method of sulfur-containing waste water comprehensive utilization and the application in nicosulfuron is produced thereof
Technical field
The present invention relates to a kind of integrated conduct method of sulfur-bearing gas phase compounds, in particular a kind of method of sulfur-containing waste water comprehensive utilization and the application in nicosulfuron is produced thereof.
Background technology
In the production process of the industries such as process hides, petrochemical industry, pharmacy, fuel, can produce a large amount of containing H 2s, SO 2, Na 2s, Na 2s 2o 3and Na 2sO 3the industrial wastewater of sulfides, is referred to as sulfur-containing waste water.Especially in recent years, the discharge capacity of sulfur-containing waste water was increasing year by year with the fast development of these industry.Sulfide in waste water is toxic, corrosivity, and tool stink, easily cause great pollution to environment, also can overflow in waste water sulfur-bearing gas phase compounds (H 2s, SO 2), give off an unpleasant smell, have a strong impact on life and the physical and mental health of people.
Nicosulfuron is a kind of high efficiency corn field herbicidal, and the process route of conventional synthesis is as follows:
Conveniently manage, aborning the reaction of each for nicosulfuron portion is divided into four workshop sections, wherein A1 workshop section need use SOCl 2, B1 workshop section need use Na 2s and S does reaction raw materials, and reaction equation is as follows:
A1 workshop section
B1 workshop section
B2 workshop section
SO is produced in course of reaction 2, H 2s, after Alkali absorption, form sulfur-containing waste water, this type of waste water directly enters Sewage Disposal if not treated, in sewage disposal process, can discharge poisonous and hazardous H 2s and SO 2gas, causes larger infringement to environmental and human health impacts.This type of wastewater treatment difficulty is comparatively large, after general employing classification of waste is collected at present, by steps such as evaporation, crystallization, filtrations, is converted into the solid waste of sulfur-bearing and processes by dangerous solid waste.There is the shortcomings such as solid waste amount is large, processing cost is high, equipment is fragile in this kind of sulfur-containing waste water processing scheme.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide the method for a kind of sulfur-containing waste water comprehensive utilization and the application in nicosulfuron is produced thereof, effectively reduce the discharge of sulphur-containing exhaust gas.
The present invention is achieved by the following technical solutions, the present invention includes following steps:
(1) containing HCl and SO 2tail gas through two-stage falling film absorption, generate Na 2sO 3solution for standby;
(2) described Na 2sO 3solution and acid reaction generate SO 2, the SO of generation 2again with containing H 2the tail gas reaction of S generates simple substance S, and obtain sulphur after filtration, filtrate is oxidized to Na further 2sO 4;
(3) excessive SO 2after alkali liquor absorption, enter HCl and SO 2tail gas two-stage falling film absorption use.
As one of preferred embodiment of the present invention, the Na of described generation 2sO 3mass concentration is 3 ~ 15%.
As one of preferred embodiment of the present invention, in described two-stage falling liquid film, all absorb with sodium hydrate aqueous solution.
As one of preferred embodiment of the present invention, the Na of described generation 2sO 3solution ph is 8 ~ 14.
As one of preferred embodiment of the present invention, described step (2) detailed process is as follows:
(21) by Na 2sO 3solution material proportion excessive 5 ~ 50% adds mixing channel, then in mixing channel, drips acid, when solution acidic, passes into containing H 2the tail gas of S;
(22) containing H 2after the tail gas absorption of S terminates, regulate mixing channel to alkalescent;
(23) mixed solution suction filtration, obtains sulphur;
(24) remaining Na in filtrate 2sO 3be oxidized to Na further 2sO 4.
As one of preferred embodiment of the present invention, in described step (21), acid is the one in hydrochloric acid, sulfuric acid and phosphoric acid.
As one of preferred embodiment of the present invention, in described step (21), in mixing channel, drip acid when realizing solution acidic, pH value is 1 ~ 6.
As one of preferred embodiment of the present invention, in described step (22), regulate mixing channel solution to be alkalescent, pH value is 8 ~ 12.
A kind of application of method in nicosulfuron is produced of sulfur-containing waste water comprehensive utilization.
By A1 workshop section containing HCl and SO 2tail gas through two-stage falling film absorption, generate Na 2sO 3for subsequent use; Na in described first order absorption 2sO 3sO is generated with acid reaction 2, the SO of generation 2with B2 workshop section containing H 2the tail gas reaction of S generates sulphur, and the sulphur of generation is used further to the production of B1 workshop section; Secondary absorbs through circulation for several times, when reaching setting concentration, enters Na 2sO 3solution tank uses.
Sulfur-containing waste water is discharged H by acidifying 2s and SO 2gas, fully contacts in confined reaction device, and reaction generates simple substance S, and obtain sulphur recovery after filtration and utilize, filtrate is oxidized to Na further 2sO 4after enter Sewage Disposal again, SO can not be discharged again 2gas, little over the SO of amount 2after alkali liquor absorption, enter HCl and SO 2tail gas secondary absorb use, work as Na 2sO 3when reaching finite concentration, enter Na 2sO 3solution tank uses.
The present invention has the following advantages compared to existing technology: the present invention is applicable to suitability for industrialized production, sulfur-containing waste water treatment effect is good, do not produce the secondary pollutions such as dangerous solid waste, cost for wastewater treatment is low, operating process is easy, the few Recovered sulphur reusable edible of equipment investment, achieves the target of the treatment of wastes with processes of wastes against one another, recycling economy.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
Detailed description of the invention
Elaborate to embodiments of the invention below, the present embodiment is implemented under premised on technical solution of the present invention, give detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
The method that sulfur-containing waste water of the present invention fully utilizes is applied in the production of nicosulfuron.
As shown in Figure 1, the retracting device of the present embodiment comprises and connects the two-stage falling film absorption system 1 of A1 workshop section, mixing channel 2, receiving slit 3, connects one-level spray column 4, the secondary spray column 5 of B2 workshop section; The Na generated after first order absorption reaction in described two-stage falling film absorption system 1 2sO 3solution enters Na 2sO 3solution liquid bath 6, the reactant liquor recycled during secondary absorbs, when reaching finite concentration, enters Na 2sO 3solution tank uses.Described mixing channel 2 is connected with receiving slit 3, the tail gas of B2 workshop section enters from the bottom of one-level spray column 4, the outlet of one-level spray column 4 connects the entrance of secondary spray column 5, the outlet of secondary spray column 5 connects receiving slit 3, mixing channel 2 is arranged respectively acid storage 7 and lye tank (vat) 8, liquid caustic soda groove 9 connects secondary spray column 5, and the reactant liquor after reaction in liquid caustic soda groove 9 is transferred in the secondary absorption system of A1 workshop section and uses.The mixed liquor reacted in rear mixing channel 2 and receiving slit 3 filters and obtains sulphur, and filtrate directly enters the Fenton oxidation workshop section of sewage disposal, by Na remaining in filtrate 2sO 3be direct oxidation into Na 2sO 4.
In order to make H 2s complete reaction, Na in the present embodiment 2sO 3all excessive 20%
The present embodiment comprises the following steps:
(1) drop in A1 still 98% thionyl chloride 133.5Kg (1.099Kmol) reaction terminate after, open two-stage falling film absorption system 1, absorb tail gas, one-level 500L water and 220L30% NaOH, secondary 500L water and 220L30% sodium hydrate aqueous solution, the insulation of A1 still terminates, stop two-stage falling film absorption system 1, first order absorption generates mass fraction 13.7%Na 2sO 3solution 927.6Kg, yield is 91.6%, Na 2sO 3solution alkaline ensures SO 2absorb completely.
(2) by 540.9Kg13.7%Na 2sO 3(folding hundred amount 74.1Kg) is put into mixing channel 2, is opened circulating pump, when to drip hydrochloric acid to solution ph be 5, has SO in mixing channel 2 2gas generates, and continues to drip hydrochloric acid, and B2 still starts to drip hydrochloric acid simultaneously, and B2 workshop section tail gas enters from the bottom of one-level spray column 4, and secondary spray column 5 connects receiving slit 3, finally regulates pH value in mixing channel 2 to be 4.After B2 still dropping hydrochloric acid terminates half an hour, in mixing channel 2, add liquid caustic soda, regulate solution ph to be 9, then be transferred in suction filtration tank by the mixed liquor in mixing channel 2 and receiving slit 3, suction filtration obtains wet sulphur, obtains sulphur 44.7Kg after drying, content 96%, yield 91.2%.
Embodiment 2
(1) A1 still throw 98% thionyl chloride 133.5Kg (1.099Kmol) reaction terminate after, open two-stage falling film absorption system 1, absorb tail gas, one-level 500L water and 220L30% NaOH, secondary 500L water and 220L30% sodium hydrate aqueous solution, the insulation of A1 still terminates, stop two-stage falling film absorption system 1, first order absorption generates mass fraction 13.7%Na 2sO 3solution 928.3Kg, yield is 92.1%, Na 2sO 3solution alkaline ensures SO 2absorb completely.
(2) by 540.9Kg13.7%Na 2sO 3(folding hundred amount 74.1Kg) is put into mixing channel 2, is opened circulating pump, when to drip hydrochloric acid to solution ph be 5, has SO in mixing channel 2 2gas generates, and continues to drip hydrochloric acid, and B2 still starts to drip hydrochloric acid simultaneously, and B2 workshop section tail gas enters from the bottom of one-level spray column 4, finally regulates pH value in mixing channel 2 to be 3.After B2 still dropping hydrochloric acid terminates half an hour, in mixing channel 2, add liquid caustic soda, regulate solution ph to be 9, then be transferred in suction filtration tank by the mixed liquor in mixing channel 2 and receiving slit 3, suction filtration obtains wet sulphur, obtains sulphur 44.9Kg after drying, content 98%, yield 93.5%.
Other embodiments are identical with embodiment 1.
Embodiment 3
(1) A1 still throw 98% thionyl chloride 133.5Kg (1.099Kmol) reaction terminate after, open two-stage falling film absorption system 1, absorb tail gas, one-level 500L water and 220L30% NaOH, secondary 500L water and 220L30% sodium hydrate aqueous solution, the insulation of A1 still terminates, stop two-stage falling film absorption system 1, first order absorption generates mass fraction 13.8%Na 2sO 3solution 929.0Kg, yield is 92.6%, Na 2sO 3solution alkaline ensures SO 2absorb completely.
(2) by 537.0Kg13.8%Na 2sO 3(folding hundred amount 74.1Kg) is put into mixing channel 2, is opened circulating pump, when to drip hydrochloric acid to solution ph be 5, has SO in mixing channel 2 2gas generates, and continues to drip hydrochloric acid, and B2 still starts to drip hydrochloric acid simultaneously, and B2 workshop section tail gas enters from the bottom of one-level spray column 4, finally regulates pH value in mixing channel 2 to be 4.After B2 still dropping hydrochloric acid terminates half an hour, in mixing channel 2, add liquid caustic soda, regulate solution ph to be 9, then be transferred in suction filtration tank by the mixed liquor in mixing channel 2 and receiving slit 3, suction filtration obtains wet sulphur, obtains sulphur 44.0Kg after drying, content 97%, yield is 90.8%.
Other embodiments are identical with embodiment 1.
Embodiment 4
(1) A1 still throw 98% thionyl chloride 133.5Kg (1.099Kmol) reaction terminate after, open two-stage falling film absorption system 1, absorb tail gas, one-level 500L water and 220L30% NaOH, secondary 500L water and 220L30% sodium hydrate aqueous solution, the insulation of A1 still terminates, stop two-stage falling film absorption system 1, first order absorption generates mass fraction 13.8%%Na 2sO 3solution 928.69Kg, yield is 92.3%, Na 2sO 3solution alkaline ensures SO 2absorb completely.
(2) by 537.0Kg13.8%Na 2sO 3(folding hundred amount 74.1Kg) is put into mixing channel 2, is opened circulating pump, when to drip hydrochloric acid to solution ph be 5, has SO in mixing channel 2 2gas generates, and continues to drip hydrochloric acid, and B2 still starts to drip hydrochloric acid simultaneously, and B2 workshop section tail gas enters from the bottom of one-level spray column 4, finally regulates pH value in mixing channel 2 to be 3.After B2 still dropping hydrochloric acid terminates half an hour, in mixing channel 2, add liquid caustic soda regulate solution ph to be 9, then the mixed liquor in mixing channel 2 and receiving slit 3 is transferred in suction filtration tank, suction filtration obtains wet sulphur, sulphur 45.7Kg is obtained, content 97%, yield 94.3% after drying.
Other embodiments are identical with embodiment 1.
Embodiment 5
(1) A1 still throw 98% thionyl chloride 133.5Kg (1.099Kmol) reaction terminate after, open two-stage falling film absorption system 1, absorb tail gas, one-level 500L water 220L30% NaOH, secondary 500L water and 220L30% sodium hydrate aqueous solution, the insulation of A1 still terminates, stop two-stage falling film absorption system 1, first order absorption generates mass fraction 13.7%Na 2sO 3solution 927.9Kg, yield is 91.8%, Na 2sO 3solution alkaline ensures SO 2absorb completely.
(2) by 540.9Kg13.7%Na 2sO 3(folding hundred amount 74.1Kg) is put into mixing channel 2, is opened circulating pump, when to drip hydrochloric acid to solution ph be 5, has SO in mixing channel 2 2gas generates, and continues to drip hydrochloric acid, and B2 still starts to drip hydrochloric acid simultaneously, and B2 workshop section tail gas enters from the bottom of one-level spray column 4, finally regulates pH value in mixing channel 2 to be 2.After B2 still dropping hydrochloric acid terminates half an hour, in mixing channel 2, add liquid caustic soda, regulate solution ph to be 9, then be transferred in suction filtration tank by the mixed liquor in mixing channel 2 and receiving slit 3, suction filtration obtains wet sulphur, obtains sulphur 46.0Kg after drying, content 98%, yield 95.8%.
Other embodiments are identical with embodiment 1.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.

Claims (9)

1. a method for sulfur-containing waste water comprehensive utilization, is characterized in that, comprise the following steps:
(1) containing HCl and SO 2tail gas through two-stage falling film absorption, generate Na 2sO 3solution for standby;
(2) described Na 2sO 3solution and acid reaction generate SO 2, the SO of generation 2again with containing H 2the tail gas reaction of S generates simple substance S, and obtain sulphur after filtration, filtrate is oxidized to Na further 2sO 4;
(3) excessive SO 2after alkali liquor absorption, enter HCl and SO 2tail gas two-stage falling film absorption use.
2. the method for a kind of sulfur-containing waste water comprehensive utilization according to claim 1, is characterized in that, the Na of described generation 2sO 3mass concentration is 3 ~ 15%.
3. the method for a kind of sulfur-containing waste water comprehensive utilization according to claim 1, is characterized in that, in described two-stage falling liquid film, all absorb with sodium hydrate aqueous solution.
4. the method for a kind of sulfur-containing waste water comprehensive utilization according to claim 1, is characterized in that, the Na of described generation 2sO 3solution ph is 8 ~ 14.
5. the method for a kind of sulfur-containing waste water comprehensive utilization according to claim 1, it is characterized in that, described step (2) detailed process is as follows:
(21) by Na 2sO 3solution material proportion excessive 5 ~ 50% adds mixing channel, then in mixing channel, drips acid, when solution acidic, passes into containing H 2the tail gas of S;
(22) containing H 2after the tail gas absorption of S terminates, regulate mixing channel to alkalescent;
(23) mixed solution suction filtration, obtains sulphur;
(24) remaining Na in filtrate 2sO 3be oxidized to Na further 2sO 4.
6. the method for a kind of sulfur-containing waste water comprehensive utilization according to claim 5, it is characterized in that, in described step (21), acid is the one in hydrochloric acid, sulfuric acid and phosphoric acid.
7. the method for a kind of sulfur-containing waste water comprehensive utilization according to claim 5, is characterized in that, in described step (21), in mixing channel, drip acid when realizing solution acidic, pH value is 1 ~ 6.
8. the method for a kind of sulfur-containing waste water comprehensive utilization according to claim 5, it is characterized in that, in described step (22), regulate mixing channel solution to be alkalescent, pH value is 8 ~ 12.
9. the application of method in nicosulfuron is produced of a sulfur-containing waste water comprehensive utilization any one of claim 1 ~ 8.
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CN110844887A (en) * 2019-11-25 2020-02-28 宜宾海翔化工有限责任公司 Method and device for treating hydrogen sulfide
CN113355527A (en) * 2021-05-11 2021-09-07 江西铜业技术研究院有限公司 Treatment method of high-sulfur smelting slag

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Publication number Priority date Publication date Assignee Title
CN110844887A (en) * 2019-11-25 2020-02-28 宜宾海翔化工有限责任公司 Method and device for treating hydrogen sulfide
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CN113355527A (en) * 2021-05-11 2021-09-07 江西铜业技术研究院有限公司 Treatment method of high-sulfur smelting slag

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