CN1063468A - From the waste water of producing anthraquinone, reclaim the method for aluminum compound - Google Patents
From the waste water of producing anthraquinone, reclaim the method for aluminum compound Download PDFInfo
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- CN1063468A CN1063468A CN 91100466 CN91100466A CN1063468A CN 1063468 A CN1063468 A CN 1063468A CN 91100466 CN91100466 CN 91100466 CN 91100466 A CN91100466 A CN 91100466A CN 1063468 A CN1063468 A CN 1063468A
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- waste water
- organic phase
- aluminum compound
- tertiary amine
- water
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Abstract
In production of anthraquinone by benzo anhydride method, produce a kind of waste water that contains anion of carboxylic group and aluminium salt.Characteristics of the present invention are exactly earlier with tertiary amine extraction decolouring, recovery aluminum compound wherein then with this waste water.This method technology not only simply but also be suitable for, the aluminum compound of recyclable non-variegation not only, and can reduce the pollution of waste water to environment.
Description
The invention belongs to the processing of waste water, relate in particular to a kind of method that from the waste water of producing anthraquinone, reclaims aluminum compound.
In production of anthraquinone by benzo anhydride method, produce a kind of waste water that contains anion of carboxylic group and aluminium salt, this waste water contains Al approximately
2O
340-50g/l, hydrogen ion concentration is 0.2-1.0mol/l and a certain amount of o-benzoylbenzoic acid.Because organic existence such as o-benzoylbenzoic acid make this waste water show brown.If with this waste water evaporative crystallization extraction aluminum ion wherein, gained aluminum compound displaing yellow or light yellow then, if aluminum ion wherein is precipitated out with the form of aluminium hydroxide with adding alkaline matter in this waste water, then gained aluminium hydroxide shows light gray-white, thereby the gained aluminum compound can not be sold as product.Cause the present most phthalic anhydride methods of China to produce the producer of anthraquinone with this discharge of wastewater.So not only environment is caused certain pollution, one ton of anthraquinone of every production simultaneously will have 0.6 ton of Al
2O
3Wave is destroyed in vain.
The object of the present invention is to provide a kind of method that from the waste water of producing anthraquinone, reclaims aluminum compound, and the aluminum compound that is reclaimed is not with variegated.
A kind of method that reclaims aluminum compound from the waste water of producing anthraquinone provided by the present invention is characterized in that comprising the steps:
(1), the waste water that will contain aluminium salt and anion of carboxylic group at room temperature fully contacts with the extracted organic phase that contains tertiary amine, and the coloring matter that contains anion of carboxylic group in this waste water is come together into organic phase.
(2), water and organic phase after will extracting leave standstill, layering then separates.
(3), the water after the extracting and separating is added the mixture that alkaline matter prepares aluminium hydroxide or prepares aluminum chloride and Tai-Ace S 150 through condensing crystal.The above-mentioned aluminum compound that reclaims after present method extraction decolouring is pure white.
The described waste water that will contain aluminium salt and anion of carboxylic group fully contacts by modes such as stirring or vibrations with the extracted organic phase that contains tertiary amine to be realized, its objective is that the coloring matter that makes aqueous phase enters organic phase to greatest extent.
Tertiary amine of the present invention is a molecular weight greater than the tertiary amines of 300 various carbon-chain structures.Comprise trioctylamine, tri-iso-octylamine, 7301, the tridecylamine of different structure has other substituent tertiary amines on trilaurylamine (Tridodecylamine and the carbochain.
Described organic phase tertiary amine add-on be 0.5%-80%(by volume), generally get final product with 2%-10%, all the other are diluent kerosene (commercially available common kerosene).
Of the present inventionly water after the extracting and separating is added alkaline matter prepare aluminium hydroxide, its alkaline matter can be ammoniacal liquor, yellow soda ash or sodium hydroxide etc.
Water after the extracting and separating of the present invention can also add aluminium ash or aluminium powder or alkaline matter in wherein, then through reaction, concentrates and obtains containing the mixture of aluminum chloride and Tai-Ace S 150 or obtain polymerize aluminum chloride and the mixture of polyaluminium sulfate.
The extracted organic phase that contains tertiary amine of the present invention can be recycled, after organic extractant phase is saturated, can add basic solution (be generally concentration be about 10% sodium hydroxide) in saturated organic phase after back extraction, organic phase is used further to cycling extraction.
Because the present invention adopts the extraction process decolouring, make decolorizing efficiency high and economical, the aluminium salt in the waste water can all reclaim and the aluminum compound outward appearance non-variegation that obtains that reclaims, easily as commodity selling.O-benzoylbenzoic acid in the waste water through the extraction after again back extraction also can reclaim.
The present invention will be described further by following examples:
Embodiment 1
Contain consisting of of anion of carboxylic group waste water: [H
+]=0.32mol/l, Al
2O
341.44g/l the waste water appearance luster is a light brown red.
Experimental technique: measure the waste water 200ml that contains anion of carboxylic group respectively and contain the composition of extracted organic phase 100ml(organic phase of tertiary amine as shown in table 1) at room temperature mixed oscillation extraction is 1 minute, behind the standing demix, water phase separated, and add 1: 1 ammoniacal liquor in water to PH=6.5, filtering-depositing, and the washing, the precipitation, then throw out is placed 70-80 ℃ dry 12.4 the gram Al(OH)
3, its appearance color is as shown in table 1.
Table 1
| Organic phase is formed (by volume) | No. 1 | No. 2 | No. 3 |
| 7,301 10%, kerosene 90% | Trioctylamine 10%, kerosene 90% | Tridecylamine 10%, kerosene 90% | |
| Gained Al (OH) 3Color | Pure white | Pure white | Pure white |
It is apparent light grey through make aluminium hydroxide with above-mentioned step without the waste water of extraction that other measures 200ml.
By The above results as can be known, all Al(OH that after tertiary amines extraction decolouring, makes)
3Be pure white, and without extracting the Al(OH that decolouring obtains)
3It but is light gray-white.
Embodiment 2
Contain consisting of of anion of carboxylic group waste water: [H
+]=0.95mol/l, Al
2O
346.19g/l the waste water appearance color is brown.
The composition of organic phase is as shown in table 2, and experimental technique is with embodiment 1, gained Al(OH)
3Color is as shown in table 2.
Table 2
| Organic phase is formed all the other kerosene of tertiary amine X% | No. 1 | No. 2 | No. 3 | No. 4 | No. 5 | |
| 7301 | X＝2 | X＝5 | X＝10 | X＝30 | X＝60 | |
| Trioctylamine | X＝2 | X＝5 | X＝10 | X＝30 | X＝60 | |
| Tridecylamine | X＝2 | X＝5 | X＝10 | X＝30 | X＝60 | |
| Gained Al (OH) 3Color | Pure white | Pure white | Pure white | Pure white | Pure white |
By the result of embodiment 1 and embodiment 2 as can be known, the add-on of tertiary amine is at 2%-80%(by volume) scope in the coloring matter in the extraction wastewater effectively, make gained aluminium hydroxide show pure white.
Embodiment 3
The waste water that contains anion of carboxylic group is with embodiment 1.Organic phase consist of (by volume), 7301:10%; Kerosene: 90%.
Experimental technique: measure the waste water 200ml and the extracted organic phase 100ml that contain anion of carboxylic group, at room temperature mixed oscillation extraction 1 minute, behind the standing demix, water intaking adopts the method for embodiment 1 to prepare aluminium hydroxide mutually, organic phase contains the waste water of anion of carboxylic group again with the aforesaid method cycling extraction, the gained water is used further to prepare aluminium hydroxide. and so circulation, gained aluminium hydroxide color is as shown in table 3.
Table 3
| Extraction times | 15 | 16 | 17 | 18 | 19 | 20 |
| Gained Al (OH) 3Color | Pure white | Pure white | Pure white | Pure white | Pure white | Pure white |
By the result of embodiment 3 as can be known, extracted organic phase can be used for the cycling extraction decolouring.
Embodiment 4
The waste water that contains anion of carboxylic group is with embodiment 1.
Experimental technique: the NaOH solution of the organic addition 10% behind the cycling extraction among the embodiment 3 20 times is at room temperature vibrated behind 1 minute standing demix, and water adds 35% sulfuric acid to [H
+]=1mol/l.Leaving standstill then then has acicular o-benzoylbenzoic acid crystal to separate out; The isopyknic aquae destillata of organic addition vibration 1 minute, standing demix is abandoned water then, adds waste water that 200ml contains anion of carboxylic group and makes lily aluminium hydroxide in organic phase with the method for experimental example 1.
By the result of embodiment 4 as can be known, extracted organic phase is renewable, and the o-benzoylbenzoic acid in the waste water is behind extracting and enriching, and is recyclable through steps such as back extractions then.
Embodiment 5
The waste water that contains anion of carboxylic group is with embodiment 1.The composition of organic phase is with embodiment 3.
Experimental technique: measure 200ml and contained the waste water of carboxyl anion and the at room temperature mixed oscillation extraction of 100ml extracted organic phase 1 minute, leave standstill, the phase of fetching water after the layering, and add solid yellow soda ash and transfer PH=2.0.Concentrate then, the white aluminium salt that obtains containing aluminum chloride and Tai-Ace S 150 is filtered in crystallization.
Other measures the waste water that 200ml contains carboxyl anion, transfers PH=2.0 with solid sodium carbonate, concentrates then, and crystallization is filtered, and gets the lurid aluminium salt that contains aluminum chloride and Tai-Ace S 150.
By the result of embodiment 5 as can be known, the aluminium salt that obtains after the extraction decolouring is much better than the aluminium salt that no bleaching obtains on appearance color.
The waste water that contains aluminium salt and anion of carboxylic group among the embodiment 1 to embodiment 5 is taken from dye processing plant, Taiyuan anthraquinone production plant.
Claims (4)
1, a kind of method that reclaims aluminum compound from the waste water of producing anthraquinone is characterised in that to comprise the steps:
(1), the waste water that will contain aluminium salt and anion of carboxylic group at room temperature fully contacts with the extracted organic phase that contains tertiary amine, and the coloring matter that contains anion of carboxylic group in this waste water is come together into organic phase,
(2), the water after will extracting leaves standstill with organic phase, layering, then separate,
(3), the water after the extracting and separating is added the mixture that alkaline matter prepares aluminium hydroxide or prepares aluminum chloride and Tai-Ace S 150 through condensing crystal.
2, the method that reclaims aluminum compound from the waste water of producing anthraquinone according to claim 1 is characterized in that described tertiary amine is a molecular weight greater than the tertiary amines of 300 various carbon-chain structures.
3, the method that reclaims aluminum compound from the waste water of producing anthraquinone according to claim 1 is characterized in that described organic phase is by 0.5%-80%(by volume) tertiary amine and surplus kerosene form.
4, the method that reclaims aluminum compound from the waste water of producing anthraquinone according to claim 3 is characterized in that described organic phase is by 2%-10%(by volume) tertiary amine and surplus kerosene form.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91100466 CN1031501C (en) | 1991-01-22 | 1991-01-22 | Process for recovery of aluminium compound from waste water during production of anthraquinone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91100466 CN1031501C (en) | 1991-01-22 | 1991-01-22 | Process for recovery of aluminium compound from waste water during production of anthraquinone |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1063468A true CN1063468A (en) | 1992-08-12 |
| CN1031501C CN1031501C (en) | 1996-04-10 |
Family
ID=4904645
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 91100466 Expired - Fee Related CN1031501C (en) | 1991-01-22 | 1991-01-22 | Process for recovery of aluminium compound from waste water during production of anthraquinone |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1031501C (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104671570A (en) * | 2014-12-24 | 2015-06-03 | 江苏同禾药业有限公司 | Method for treating aluminum-containing wastewater in preparation process of 6-oxo-8-chloro ethyl caprylate |
| CN105836865A (en) * | 2016-06-04 | 2016-08-10 | 江阴市长江化工有限公司 | Process for preparing poly aluminum chloride |
| CN106800346A (en) * | 2017-02-07 | 2017-06-06 | 泰山医学院 | A kind of method of integrated treatment containing alchlor industrial wastewater |
-
1991
- 1991-01-22 CN CN 91100466 patent/CN1031501C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104671570A (en) * | 2014-12-24 | 2015-06-03 | 江苏同禾药业有限公司 | Method for treating aluminum-containing wastewater in preparation process of 6-oxo-8-chloro ethyl caprylate |
| CN105836865A (en) * | 2016-06-04 | 2016-08-10 | 江阴市长江化工有限公司 | Process for preparing poly aluminum chloride |
| CN106800346A (en) * | 2017-02-07 | 2017-06-06 | 泰山医学院 | A kind of method of integrated treatment containing alchlor industrial wastewater |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1031501C (en) | 1996-04-10 |
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