CN1040012A - The recovery method of the processing of vat powder waste liquid and S-WAT and sodium-chlor - Google Patents

The recovery method of the processing of vat powder waste liquid and S-WAT and sodium-chlor Download PDF

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CN1040012A
CN1040012A CN 89102534 CN89102534A CN1040012A CN 1040012 A CN1040012 A CN 1040012A CN 89102534 CN89102534 CN 89102534 CN 89102534 A CN89102534 A CN 89102534A CN 1040012 A CN1040012 A CN 1040012A
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waste liquid
sodium
chlor
wat
vat powder
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CN1014695B (en
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陶文典
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LAOHEKOU CITY PETROLEUM-CHEMICAL GENERAL PLANT
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LAOHEKOU CITY PETROLEUM-CHEMICAL GENERAL PLANT
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Abstract

The present invention relates to the method that a kind of zinc method is produced the processing of vat powder waste liquid and reclaim S-WAT and sodium-chlor from waste liquid.This method is direct logical sulfurous gas in waste liquid, controlled temperature 40-60 ℃, when waste liquor PH=5-6, return neutralization with former alkaline waste liquor, and make its pH=9-10.Then waste liquid is carried out single vaporization and get S-WAT, filtrate is carried out double evaporation-cooling and is got sodium-chlor, and the mother liquor after the filtration returns not sewage effluent of double evaporation-cooling, does not have secondary pollution.Gained sodium-chlor is used for salting-out procedures, does not influence the quality standard and the yield of vat powder.

Description

The recovery method of the processing of vat powder waste liquid and S-WAT and sodium-chlor
The present invention relates to the method that a kind of zinc method is produced the processing of vat powder (Sodium Hydrosulphite) waste liquid and reclaim S-WAT and sodium-chlor from waste liquid.
The process that the zinc method is produced vat powder is:
(1) the zinc powder slurry is reacted into low pressure zinc sulfite with sulfurous gas:
(2) neutralization and metathesis: use in the sodium hydroxide and low pressure zinc sulfite solution, low pressure zinc sulfite is transformed into Sodium Hydrosulphite simultaneously.
(3) saltout: the aqueous solution of vat powder is saltoutd with sodium-chlor and is got vat powder.
When producing vat powder with aforesaid method, 1 ton of vat powder of every production will produce 9m 3Waste liquid, wherein cold waste liquid 8m 3, thermal effluent 1m 3The composition of cold waste liquid and content are: NaCl20%, NaOH5%, Na 2S 2O 4(Sodium Hydrosulphite vat powder) 2%Na 2SO 32%, Na 2S0.5%, the composition of thermal effluent and content are: Na 2S 3-4%, other composition and cold waste liquid are basic identical.
The waste liquid that produces is because Na wherein 2S 2O 4In storage process, decompose institute extremely, so, NaOH in the waste liquid and Na 2S 2O 4Content obviously descends, and Na 2S content obviously raises.Can cause severe contamination to environment behind this discharging of waste liquid that contains alkali and a large amount of reducing substanceses, and useful matter is wherein utilized rationally and is wasted.
Present domestic producer's great majority with zinc method production vat powder are that waste liquid is directly emitted, minority producer is to reclaim NaCl behind the waste liquid direct evaporation to the treatment process of waste liquid, the mother liquor that is produced is a lower concentration NaOH solution, returns to be used in the production and the operation use.The shortcoming of this method is that waste liquid need leave standstill more than 24 hours before carrying out evaporation process, so that sedimentation microlite vat powder (Na wherein 2S 2O 4, 2H 2O), in the process of leaving standstill, have a certain amount of vat powder to decompose, and vat powder and sodium hydroxide complete reaction generate S-WAT and sodium sulphite in the high temperature evaporation process.(3Na 2S 2O 4+ NaOH → 5Na 2SO 3+ Na 2S+3H 2O) about 2% vat powder decomposes the NaOH that needs consumption about 2% fully in the waste liquid, thereby makes the content of NaOH in the mother liquor very low, makes again and contains a large amount of Na among the NaCl 2SO 3(Na in evaporative process 2SO 3Separate out prior to NaCl.) thisly contain a large amount of Na 2SO 3NaCl return use in the production and can make Na in the waste liquid 2SO 3Thereby the higher vat powder yield that makes of content is lower.Make Na in the waste liquid 2SO 3Content raise, this waste liquid is evaporated again reclaims NaCl, Na among the NaCl as a result 2SO 3Content can further raise, cause vicious cycle, and the rate of recovery of this method sodium-chlor and S-WAT is very low, the high deficiency in economic performance of cost.The NaCl of while waste liquid recovery for the third time is because Na wherein 2SO 3Content is too high, can not be used for vat powder production, thereby waste liquid have to discharge, and causes for the second time and pollutes.
The method that the present invention proposes can all be recycled the material in the waste liquid, does not discharge waste liquid, does not have secondary pollution, and the sodium-chlor Central Asia sodium sulphate content that is reclaimed is very low, can directly return in the salt operation and use, and does not influence the yield and the quality standard of vat powder.
According to the present invention waste liquid is directly fed SO 2, make the PH of waste liquid reach acid, preferably PH is 5-6, temperature preferably is controlled at 40-60 ℃ of NaOH and the SO in the waste liquid at 10-90 ℃ 2Reaction all generates Na 2SO 3And NaHSO 3, also when the pH value of waste liquid reached neutral or acid, decomposition became Na to the vat powder in the waste liquid fully 2SO 3Na in the waste liquid 2S and SO 2Reaction generates Na 2SO 3, then,, make its PH to alkalescence with the alkaline waste liquor neutralization, preferably PH=9-10 makes NaHSO 3All will turn to Na 2SO 3
According to method of the present invention, only contain Na in the treated waste liquid 2SO 3With two kinds of salt of NaCl, utilize Na 2SO 3With the different solubilities of two kinds of salt of NaCl in water, carry out twice evaporation, Na 2SO 3At first separate out, filter Na 2SO 3Filtrate is carried out the evaporation second time again, obtains NaCl after the filtration, and mother liquor returns and carries out circulating and evaporating, thereby has removed sewage discharge, Na among the NaCl that obtains 2SO 3Content seldom, directly return quality and yield that salting-out procedures is used does not influence vat powder.Because Na in evaporative process 2SO 3Separate out prior to NaCl, thereby the Na among the NaCl 2SO 3Content can not increase, thereby has got rid of vicious cycle.
Main chemical reactions has:
Feeding SO 2Process in react and 1. and 2. carry out simultaneously, but under the excessive situation of SO promptly in acidic medium the reaction end of NaOH be Na 2SO 3With suitable NaHSO 3; Use in the excessive slightly alkaline waste liquor then and NaHSO 3, make it be converted into Na fully 2SO 3; 3. reaction is Na 2S 2O 4Decomposition reaction in neutrality or acidic solution, the Na of a molecule 2S 2O 4Decompose the SO that needs to consume a molecule 2, but produced the SO of 2 molecules after decomposing again 2, aggravate Na simultaneously 2S 2O 4Decomposition, the acid of solution improved rapidly, 4. reaction is the Na that self exists in the waste liquid 2S and Na 2S 2O 4Decompose the Na that produces 2S and excessive SO 2The Na that reaction is produced 2SO 3And H 2The reaction of S; 5. reaction is Na 2S 2O 4The decomposition reaction that the waste liquid shelf-time is long or temperature is too high (50 ℃) takes place in basic solution.
The present invention has following advantage and positively effect:
1. the main component in the waste liquid all is converted into S-WAT and sodium-chlor, has realized the living comprehensive utilization of producing the vat powder waste liquid of zinc method.
2. the present invention has realized the ideal process of waste liquid, and only product does not produce " three wastes ".
3, utilize method of the present invention, the sodium hydride that returns thing from waste liquid directly recycles in the retrieval system, can not influence the quality standard and the yield of vat powder, and the S-WAT that (seeing attached list 1) reclaims simultaneously reaches the raw product standard.
Figure 891025340_IMG2
Annotate: the vat powder quality standard is 85.5%.
4, economic benefit and obvious social benefit, subordinate list 2 is for producing the economic benefit after 1 ton of vat powder institute removal waste fluid is handled with method of the present invention.
Figure 891025340_IMG3
Be that one ton of vat powder of every production can reduce cost 804 yuan.
Technological process of the present invention as shown in the figure, description of drawings is as follows:
Neutralizer is waste liquid and SO 2Reaction gained solution.
Filtrate is single vaporization after-filtration gained solution.
Mother liquor is a double evaporation-cooling after-filtration gained solution.
Embodiment
1, the neutralization of waste liquid: get waste liquid 8.3m 3Put into 11m 3Reactor in stir and to feed SO down 2Hydrogen precursor reactant temperature is controlled at 40-60 ℃, normal pressure control reaction end P=5-6, and at this moment, the sodium hydroxide in the solution all reacts with sulfurous gas, and vat powder also decomposes fully, and 0.7-0.8m is used in sodium sulphite while and sulfurous gas reaction then 3Alkaline waste liquor neutralizes and regulates PH=9-10.Make the sodium pyrosulfate in the solution all be converted into S-WAT, because waste liquid itself is the saturated solution of sodium salt, so terminal point has a small amount of S-WAT to separate out.
2, single vaporization gets S-WAT, and the resulting solution that will neutralize carries out vacuum-evaporation, and temperature is controlled at 80-90 ℃, and the 35-45% that evaporated volume accounts for cumulative volume filters, and promptly is less than net weight 1.42T content and is 61.2% thick S-WAT.
3, double evaporation-cooling: the filtrate of evaporation is carried out the secondary vacuum evaporation for the first time, vaporization temperature is controlled at 80-90 ℃, filters, and gets the wet sodium-chlor (moisture 11%) of 1.72T and can directly return the independent or mixing of salting-out procedures, the content that uses S-WAT wherein is below 2%, and mother liquor returns double evaporation-cooling.

Claims (4)

1, a kind of method that reclaims sodium-chlor and S-WAT from zinc method production vat powder waste liquid is characterized in that the directly logical sulfurous gas of waste liquid; Control reaction temperature 40-60 ℃, when the PH=5-6 of waste liquid, transfer the waste liquid of PH=5-6 with alkaline waste liquor, make after its PH=9-10, handled waste liquid is carried out single vaporization get S-WAT, filter, filtrate is carried out double evaporation-cooling get sodium-chlor and mother liquor.
2,, it is characterized in that double evaporation-cooling filters the mother liquid obtained double evaporation-cooling that returns in back and uses according to the method for described recovery sodium-chlor of claim 1 and S-WAT.
3, according to the method for described recovery sodium-chlor of claim 1 and S-WAT, the salting-out procedures of its characterization when gained sodium-chlor behind double evaporation-cooling can directly return the production vat powder goes to use.
4,, it is characterized in that the volume of evaporation accounts for the 35-45% of cumulative volume when the S-WAT of evaporation recovery for the first time according to the method for described recovery sodium-chlor of claim 1 and S-WAT.
CN 89102534 1989-04-18 1989-04-18 Process for producing safety powder by zinc method and method for recovering sodium sulfite and common salt from waste liguor Expired CN1014695B (en)

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CN 89102534 CN1014695B (en) 1989-04-18 1989-04-18 Process for producing safety powder by zinc method and method for recovering sodium sulfite and common salt from waste liguor

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CN 89102534 CN1014695B (en) 1989-04-18 1989-04-18 Process for producing safety powder by zinc method and method for recovering sodium sulfite and common salt from waste liguor

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CN1014695B CN1014695B (en) 1991-11-13

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103694101A (en) * 2013-11-07 2014-04-02 济南大学 Comprehensive utilization method of sodium hydrosulfite waste residue
CN103755048A (en) * 2013-12-30 2014-04-30 中盐安徽红四方股份有限公司 New sodium hydrosulfite wastewater treatment method
CN103754896A (en) * 2013-12-21 2014-04-30 中盐安徽红四方股份有限公司 Method for extracting mirabilite from sodium hydrosulfite wastewater
CN105016312A (en) * 2015-07-08 2015-11-04 湖南龙盛环保有限公司 Recycling utilization method for sulfur-contained waste material in production of sodium hydrosulfite
CN105502769A (en) * 2015-12-29 2016-04-20 河北诚信九天医药化工有限公司 Method for recycling esterification acid wastewater produced in ethyl cyanoacetate production
CN110304639A (en) * 2019-07-10 2019-10-08 连云港莱亚化学有限公司 A kind of method of purification of ortho-sulfonic acid sodium benzaldehyde by-product salt

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103694101A (en) * 2013-11-07 2014-04-02 济南大学 Comprehensive utilization method of sodium hydrosulfite waste residue
CN103694101B (en) * 2013-11-07 2015-08-19 济南大学 A kind of method of comprehensive utilization of sodium hydrosulfite waste residue
CN103754896A (en) * 2013-12-21 2014-04-30 中盐安徽红四方股份有限公司 Method for extracting mirabilite from sodium hydrosulfite wastewater
CN103754896B (en) * 2013-12-21 2016-06-15 中盐安徽红四方股份有限公司 A kind of method extracting Natrii Sulfas in sodium hydrosulfite wastewater
CN103755048A (en) * 2013-12-30 2014-04-30 中盐安徽红四方股份有限公司 New sodium hydrosulfite wastewater treatment method
CN105016312A (en) * 2015-07-08 2015-11-04 湖南龙盛环保有限公司 Recycling utilization method for sulfur-contained waste material in production of sodium hydrosulfite
CN105502769A (en) * 2015-12-29 2016-04-20 河北诚信九天医药化工有限公司 Method for recycling esterification acid wastewater produced in ethyl cyanoacetate production
CN105502769B (en) * 2015-12-29 2018-05-08 河北诚信九天医药化工有限公司 A kind of method of esterified acid waste water in recycling treatment cyan-acetic ester production
CN110304639A (en) * 2019-07-10 2019-10-08 连云港莱亚化学有限公司 A kind of method of purification of ortho-sulfonic acid sodium benzaldehyde by-product salt
CN110304639B (en) * 2019-07-10 2022-04-08 浙江宏达化学制品有限公司 Purification method of sodium o-sulfonate benzaldehyde byproduct salt

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