CN106745602A - The method for preparing aluminium polychloride using spent acid and aluminium salt waste liquid - Google Patents
The method for preparing aluminium polychloride using spent acid and aluminium salt waste liquid Download PDFInfo
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- CN106745602A CN106745602A CN201611183147.4A CN201611183147A CN106745602A CN 106745602 A CN106745602 A CN 106745602A CN 201611183147 A CN201611183147 A CN 201611183147A CN 106745602 A CN106745602 A CN 106745602A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/48—Halides, with or without other cations besides aluminium
- C01F7/56—Chlorides
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
- C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a kind of method that utilization spent acid and aluminium salt waste liquid prepare aluminium polychloride.The method is with 4, the waste hydrochloric acid and aluminium salt waste liquid produced in 4' dichloro sulfoxide production processes are raw material, organic matter chlorobenzene and 4 are removed by extractant of dichloromethane, 4' dichloro sulfoxides, then add a certain amount of calcium aluminate powder to be reacted in aqueous, aluminium content, basicity and the pH value of mixed liquor are adjusted by adding a certain proportion of water.After reaction terminates, the consumption of calcium aluminate powder is 18% the 25% of waste hydrochloric acid and aluminium salt waste liquid quality.Waste hydrochloric acid and aluminium salt waste liquid and the temperature of calcium aluminate powder reaction are 100 105 DEG C, and the time of reaction is 23 hours, the aluminum oxide of aluminium polychloride fluid product（Al2O3Meter）Mass fraction be 10% 12%, basicity is 65% 75%, and pH value is 35.The inventive method can effectively remove 4, chlorobenzene and 4 in the waste hydrochloric acid and aluminium salt waste liquid that are produced in 4' dichloro sulfoxide production processes, the organic matters such as 4' dichloro sulfoxides, are a kind of pollution-free, environmental protection production technologies, with good economic benefit and social benefit.
Description
Technical field
The present invention relates to a kind of preparation method of aluminium polychloride, aluminium polychloride is prepared in particular with spent acid and aluminium salt waste liquid
Method.
Background technology
Aluminium polychloride (Poly aluminum Chloride) code name PAC, is between AlCl3With Al (OH)3Between one
Water-soluble inorganic high molecular polymer is planted, chemical general formula is [Al2(OH)nCl6-n]mWherein m represents extent of polymerization, and n represents that PAC is produced
The neutral degree of product.The structure of aluminium polychloride is made up of the changeable polycarboxy complex compound of form, is inhaled with stronger bridge formation
Attached performance, in hydrolytic process, with condensing, the physical and chemical process such as adsorbs and precipitates.Flocculation sediment speed is fast, is applicable
PH range is wide, to pipe-line equipment non-corrosiveness, purifying water effect substantially, can chromaticness SS, COD, BOD and arsenic effectively in branch water removal,
The heavy metal ion such as mercury, the product is widely used in drinking water, industrial water and sewage treatment area.
4,4'- dichloro sulfoxides are that sulfoxide oxidation method prepares 4, the intermediate products of 4 '-dichloro diphenyl sulfone, by protochloride
Sulfone and chlorobenzene are in catalyst AlCl3Friedel-Crafts reaction preparation is carried out under effect, the byproduct hydrogen chloride gas of generation can be carried secretly on a small quantity
Raw material chlorobenzene and thionyl chloride, waste hydrochloric acid is recycled into by recirculated water absorption tower, and residual exhaust generates salt with alkali reaction immediately.Will
Friedel-Crafts reaction material is put into another reactor and adds water and is hydrolyzed, and now alchlor is hydrolyzed reaction, generates hydrogen chloride
Gas, can carry a small amount of chlorobenzene secretly, and waste hydrochloric acid is recycled into by recirculated water absorption tower.Reaction generation 4,4'- dichloro sulfoxides
Crystal, by press filtration, obtains sulfoxide first product, and liquid contains chlorobenzene and aluminium hydroxide and the alchlor aqueous solution, by stratification,
Water is mutually mainly the acidic aqueous solution of aluminium hydroxide and alchlor, contains a small amount of chlorobenzene and 4,4'- dichloro sulfoxide.As
Substantial amounts of spent acid and aluminium salt waste liquid are produced in 4,4'- dichloro sulfoxide production processes, how to prevent environmental pollution, realize spent acid
Environmental protection treatment and comprehensive utilization with waste liquid, are that sulfoxide oxidation method prepares 4, and 4 '-dichloro diphenyl sulfone chemical technology is badly in need of what is solved
Problem.
The content of the invention
The present invention provides a kind of method that utilization spent acid and aluminium salt waste liquid prepare aluminium polychloride, and it is directed to 4,4'- dichloros two
Substantial amounts of spent acid and aluminium salt waste liquid are produced in benzene sulfoxide production process, environmental protection treatment and the comprehensive utilization of spent acid and waste liquid is realized,
Be it is a kind of turn waste into wealth, the production technology of anti-pollution recycling, with good economic benefit and social benefit.
The present invention is achieved by the following technical solutions
The method that a kind of utilization spent acid of the present invention and aluminium salt waste liquid prepare aluminium polychloride, with spent acid and aluminium salt waste liquid as raw material,
It is to comprise the following steps, 1）Abstraction impurity removal, extractant is added to the spent acid and aluminium salt waste liquid raw material, agitated, extraction,
Standing separation removal of impurities, organics removal chlorobenzene and 4,4'- dichloro sulfoxide organic phase, obtain water phase；2）Preparing polymeric aluminium chloride, to
A certain amount of aluminic acid salt fines are added in above-mentioned water phase, added water, heated, stirring reaction, after reaction terminates, obtain water regulation mixing
Liquid；Water regulation mixed liquor is stood, sedimentation obtains supernatant liquor as water treatment agent aluminium polychloride fluid product；The extraction
Solvent is two chloroalkyl cpds, and the aluminic acid salt fines are calcium aluminate powder and/or aluminic acid magnesium powder.
Further, the spent acid and aluminium salt waste liquid raw material are produced with 4,4'- dichloro sulfoxide production processes
Waste hydrochloric acid and aluminium salt waste liquid are raw material；The chloroalkyl cpd of the extractant two is dichloromethane.
Preferably, it is that the spent acid is waste hydrochloric acid, controls the HCl contents of the waste hydrochloric acid for 22-25wt%, aluminium salt waste liquid
Middle aluminium composition is 6.0-7.0 wt %；It is spent acid and the 15- of aluminium salt waste liquid quality to control the consumption of the extractant
25wt%, at twice abstraction impurity removal.
Further, it is that to control the consumption of the calcium aluminate powder be waste hydrochloric acid and the 18-25 wt % of aluminium salt waste liquid quality.
Further, it is that the temperature for controlling the spent acid and aluminium salt waste liquid of the water phase to be reacted with aluminic acid salt fines is 100-105
DEG C, it is spent acid and the 20%-30% of aluminium salt waste liquid quality to control the amount for adding water, and it is 2-3 hours to control the reaction time；Control stands heavy
The time of drop is 48-72 hours.
Preferably, be control the aluminium polychloride fluid product aluminum oxide with Al2O3The mass fraction content of meter is
10-12 wt %, basicity is 65-75%, and pH value is 3-5.
It is furthermore preferred that being mass fraction≤0.1% of the insoluble matter of aluminium polychloride fluid product.
The inventive method can effectively remove the waste hydrochloric acid and aluminium salt waste liquid produced in 4,4'- dichloro sulfoxide production processes
In chlorobenzene and the organic matter such as 4,4'- dichloro sulfoxide, the recyclable recycling of extractant, be a kind of pollution-free, green
The production technology of environmental protection.
Specific embodiment
With reference to specific embodiment, the present invention is described in further detail；Each component described in embodiment be quality or
Mass percent.
Embodiment 1
400g aluminium salt waste liquids aluminium content is taken for 7.0% and 50g waste hydrochloric acids, it is 24% to control the HCl contents in waste hydrochloric acid, be put into anti-
Answer in bottle, add dichloromethane 40ml, stirring extraction 30 minutes separates organic phase after stratification；Dichloromethane is added again
40ml, stirring extraction 30 minutes, separates organic phase after stratification, i.e. removal contains organic matter chlorobenzene and 4,4'- dichloro
The organic phase of sulfoxide, obtains water phase.Organic phase is merged, after dichloromethane Distillation recovery reuse, a small amount of residue be chlorobenzene and
4,4'- dichloro sulfoxides.Calcium aluminate powder 90g is added in Xiang Shuixiang, its quality is that content is 48%, stirring reaction, and is added
100g water, is heated to 100-105 DEG C, stirring reaction 2 hours.After reaction terminates, water regulation mixed liquor is obtained, water is adjusted into mixed liquor
Stand, settle 2 days, obtain supernatant liquor, supernatant liquor is the aluminium polychloride fluid product of water treatment agent.The present embodiment is given birth to
The indexs such as the quality of alumina fraction and basicity of the aluminium polychloride product of product are detected that table 1, detection method is referred to《GB/
T 22627-2014 water treatment agent polyaluminium chlorides》.
Table 1
| Inspection project | Assay |
| Aluminum oxide（Al2O3Meter）Mass fraction % | 11.2% |
| Basicity % | 72.2% |
| The mass fraction % of insoluble matter | 0.05% |
| PH value（The 10g/L aqueous solution） | 3.0 |
| Density（20℃）g/cm3 | 1.268 |
Explanation：The aluminium polychloride product of the inventive method production, reaches the quality requirement of water treatment agent.Following embodiments are removed and said
Outside bright, remaining end explanation part is identical with production method described in embodiment 1.
Embodiment 2
Take 400 Kg aluminium salts waste liquids (aluminium content is 6.5 %) and 55 Kg waste hydrochloric acids (HCl contents are 24.5%) are put into reactor
In, dichloromethane 40L is added, stirring extraction 30 minutes separates organic phase after stratification；Dichloromethane 40L is added again, is stirred
Extraction 30 minutes is mixed, organic phase is separated after stratification.Organic phase is merged, is reused after dichloromethane Distillation recovery, it is few
Amount residue is chlorobenzene and 4,4'- dichloro sulfoxides.Water is added to the Kg of calcium aluminate powder 110 (content is 48%), stirring reaction,
And 100 Kg water are added, and 100-105 DEG C is heated to, stirring reaction 3 hours is discharged after tail gas clean-up.After reaction terminates, will mix
Liquid standing sedimentation 3 days, supernatant liquor is water treatment agent aluminium polychloride fluid product.To the polyaluminium chloride product oxygen for having produced
Change the indexs such as aluminium mass fraction and basicity to be detected, table 2, detection method reference《GB/T 22627-2014 water treatment agents
Polyaluminium chloride》.
Table 2
| Inspection project | Assay |
| Aluminum oxide（Al2O3Meter）Mass fraction % | 11.8% |
| Basicity % | 74.5% |
| The mass fraction % of insoluble matter | 0.06% |
| PH value（The 10g/L aqueous solution） | 4.0 |
| Density（20℃）g/cm3 | 1.262 |
Embodiment 3
Take 2000 Kg aluminium salts waste liquids (aluminium content is 6.7 %) and 250 Kg waste hydrochloric acids (HCl contents are 23.5%) are put into reaction
In kettle, dichloromethane 120L is added, stirring is extracted 30 minutes, and stratification separates organic phase after 1 hour；Dichloromethane is added again
Alkane 120L, stirring extraction 30 minutes, stratification separates organic phase after 1 hour.Organic phase is merged, dichloromethane Distillation recovery
After reuse, residue be chlorobenzene and 4,4'- dichloro sulfoxide.Water is added to the Kg of calcium aluminate powder 450 (content is 48%),
Stirring reaction, and 600 Kg water are added, 100-105 DEG C is heated to, stirring reaction 3 hours is discharged after tail gas clean-up.Reaction terminates
Afterwards, by mixed liquor standing sedimentation 3 days, supernatant liquor is water treatment agent aluminium polychloride fluid product.To the polychlorostyrene for having produced
Change the indexs such as aluminium product quality of alumina fraction and basicity to be detected, table 3, detection method reference《GB/T 22627-2014
Water treatment agent polyaluminium chloride》.
Table 3
| Inspection project | Assay |
| Aluminum oxide（Al2O3Meter）Mass fraction % | 10.5% |
| Basicity % | 67.5% |
| The mass fraction % of insoluble matter | 0.05% |
| PH value（The 10g/L aqueous solution） | 4.0 |
| Density（20℃）g/cm3 | 1.255 |
The present invention is to utilize the waste hydrochloric acid and the acid aluminium salt containing organic matter produced in 4,4 '-dichloro sulfoxide production process
The method that waste liquid prepares aluminium polychloride.Its prepare aluminium polychloride product, meet the requirement of water treatment agent, realize spent acid and
The environmental protection treatment of waste liquid and comprehensive utilization.
Claims (6)
1. a kind of method that utilization spent acid and aluminium salt waste liquid prepare aluminium polychloride, with spent acid and aluminium salt waste liquid as raw material, it is special
It is to comprise the following steps to levy, 1）Abstraction impurity removal, extractant is added to the spent acid and aluminium salt waste liquid raw material, agitated, extraction,
Standing separation removal of impurities, removes chlorobenzene containing organic matter and 4,4'- dichloro sulfoxide organic phase, obtains water phase；2）Preparing polymeric aluminium chloride,
To a certain amount of aluminic acid salt fines are added in above-mentioned water phase, add water, heat, stirring reaction, after reaction terminates, obtaining water regulation mixing
Liquid；Water regulation mixed liquor is stood, sedimentation obtains supernatant liquor as water treatment agent aluminium polychloride fluid product；The extraction
Solvent is two chloroalkyl cpds, and the aluminic acid salt fines are calcium aluminate powder and/or aluminic acid magnesium powder.
2. the method for preparing aluminium polychloride using spent acid and aluminium salt waste liquid according to claim 1, it is characterized in that described useless
Acid and aluminium salt waste liquid raw material are the waste hydrochloric acid and aluminium salt waste liquid produced with 4,4'- dichloro sulfoxide production processes as raw material；
The chloroalkyl cpd of the extractant two is dichloromethane.
3. the method that utilization spent acid according to claim 1 or claim 2 and aluminium salt waste liquid prepare aluminium polychloride, it is characterized in that described
Spent acid is waste hydrochloric acid, controls the HCl contents of the waste hydrochloric acid for 22-25 wt%, and aluminium composition is 6.0-7.0 in aluminium salt waste liquid
wt %；The consumption for controlling the extractant is the 15-25 wt% of spent acid and aluminium salt waste liquid quality, at twice abstraction impurity removal.
4. the method for preparing aluminium polychloride using spent acid and aluminium salt waste liquid according to claim 1, it is characterized in that control institute
It is waste hydrochloric acid and the 18-25 wt % of aluminium salt waste liquid quality to state the consumption of calcium aluminate powder.
5. the method for preparing aluminium polychloride using spent acid and aluminium salt waste liquid according to claim 1, it is characterized in that control institute
The spent acid and aluminium salt waste liquid and the temperature of aluminic acid salt fines reaction for stating water phase are 100-105 DEG C, and it is spent acid and aluminium to control the amount for adding water
The 20-30% of bisulfate waste liquor quality, the reaction time is 2-3 hours；The time for controlling standing sedimentation is 48-72 hours.
6. the method for preparing aluminium polychloride using spent acid and aluminium salt waste liquid according to claim 1, it is characterized in that control institute
The aluminum oxide of aluminium polychloride fluid product is stated with Al2O3The mass fraction of meter is 10-12 wt %, and basicity is 65-75%, pH
It is 3-5 to be worth.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109019740A (en) * | 2018-07-31 | 2018-12-18 | 大连理工大学 | A kind of sulfolane wastewater treatment method |
| CN109781913A (en) * | 2018-12-07 | 2019-05-21 | 江苏永葆环保科技有限公司 | The detection method of organic matter in a kind of acid pickle |
| CN111747435A (en) * | 2020-07-08 | 2020-10-09 | 宁夏蓝田农业开发有限公司 | Method for preparing flocculant by using oxadiargyl byproduct |
| WO2021094538A1 (en) * | 2019-11-13 | 2021-05-20 | Basf Se | A process for working up water containing 4,4'-dichlorodiphenyl sulfoxide and/or 4,4'-dichlorodiphenyl sulfone as impurities |
| CN113247996A (en) * | 2021-02-08 | 2021-08-13 | 江苏扬农化工股份有限公司 | Method for treating aluminum trichloride wastewater |
| CN114702054A (en) * | 2022-04-13 | 2022-07-05 | 衡阳市建衡实业有限公司 | Production process of high-purity polyaluminum chloride |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109019740A (en) * | 2018-07-31 | 2018-12-18 | 大连理工大学 | A kind of sulfolane wastewater treatment method |
| CN109781913A (en) * | 2018-12-07 | 2019-05-21 | 江苏永葆环保科技有限公司 | The detection method of organic matter in a kind of acid pickle |
| WO2021094538A1 (en) * | 2019-11-13 | 2021-05-20 | Basf Se | A process for working up water containing 4,4'-dichlorodiphenyl sulfoxide and/or 4,4'-dichlorodiphenyl sulfone as impurities |
| CN114728818A (en) * | 2019-11-13 | 2022-07-08 | 巴斯夫欧洲公司 | Method for treating water containing 4,4 '-dichlorodiphenyl sulfoxide and/or 4, 4' -dichlorodiphenyl sulfone as impurities |
| CN111747435A (en) * | 2020-07-08 | 2020-10-09 | 宁夏蓝田农业开发有限公司 | Method for preparing flocculant by using oxadiargyl byproduct |
| CN111747435B (en) * | 2020-07-08 | 2022-10-25 | 宁夏蓝田农业开发有限公司 | Method for preparing flocculant by oxadiargyl byproduct |
| CN113247996A (en) * | 2021-02-08 | 2021-08-13 | 江苏扬农化工股份有限公司 | Method for treating aluminum trichloride wastewater |
| CN114702054A (en) * | 2022-04-13 | 2022-07-05 | 衡阳市建衡实业有限公司 | Production process of high-purity polyaluminum chloride |
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