CN1052291A - Method with aluminium wastewater system exsiccated ammonium alum - Google Patents
Method with aluminium wastewater system exsiccated ammonium alum Download PDFInfo
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- CN1052291A CN1052291A CN 89109109 CN89109109A CN1052291A CN 1052291 A CN1052291 A CN 1052291A CN 89109109 CN89109109 CN 89109109 CN 89109109 A CN89109109 A CN 89109109A CN 1052291 A CN1052291 A CN 1052291A
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- ammonium alum
- exsiccated ammonium
- water
- friedel
- aluminium
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Abstract
The present invention is that the used aluminum chloride of friedel-crafts (Friedel-Crafts) reaction provides the method for producing exsiccated ammonium alum that reclaims.Product purity reaches more than 99.5%.
Produce exsiccated ammonium alum with the inventive method, do not use bauxite, ammonium sulfate, and come in the Ford reaction sulfur waste acid in the aluminum chloride and acidifying decomposition course to recycle Fred-gram.The rate of recovery of aluminium can reach more than 85%, and the sulfuric acid consumption is than bauxite technology decline 10-20%.The present invention also makes the wastewater produced easier processing of Friedel-Crafts reaction.So the present invention also is one of environment protection method.
Description
A kind of manufacture method of exsiccated ammonium alum.The invention relates to the method that used aluminum chloride is produced exsiccated ammonium alum by further utilization in friedel-crafts in the organic synthesis (Friedel-Crafts) reaction process.
At present, exsiccated ammonium alum is with bauxite (salic 40%), and sulfuric acid, ammonium sulfate are that basic material prepares.Need a large amount of valuable aluminum smelting industry raw material bauxite that consume.And the catalyzer aluminum chlorides that use in a large number in Friedel-Crafts reaction production chemical product process are but further effectively utilized.Warp is to U.S. Dialog system world patent document 351.350(1963-1989) scan search, find that the patent consistent with the meaning of the question of the present invention exists.
The present invention makes the method for exsiccated ammonium alum, and having avoided former is the existing complex process of preparation technology of raw material with bauxite, ammonium sulfate, production cost height, the defective of generation waste residue, waste water.The objective of the invention is to used aluminum chloride in the Friedel-Crafts reaction is utilized once more,, replace the used bauxite of original technology as the aluminium source.To aluminum chlorides a large amount of behind the Veux-psoriasis reaction, under acidic conditions, aluminium is changed in the waste water at present.The present invention also aims to that the sulfuric acid that changes in the waste water that uses is decomposed in acidifying in the reaction and carry out the part utilization.Simultaneously, make the acid waste water amount that is produced in the Veux-psoriasis reaction reduce, and more easily handle, help environment protection.
The inventive method is to utilize useless aluminum chloride finally to be situated between by sulfuric acid, water institute water and change aluminium and sulfuric acid in the waste water (mother liquor water) over to, prepares exsiccated ammonium alum with ammonia react.For example utilize the method for the aluminum chloride manufacturing exsiccated ammonium alum in friedel-crafts (Friedel-Crafts) reaction.Implementation step is:
1, gets decomposition nut liquid water behind the Friedel-Crafts reaction, isolate the organism of carrying secretly, make aluminium ion concentration C
8Be the 0.8-2.5 mol, the present invention's technical requirements preferably is C
8Be the 1.15-1.5 mol;
2, will meet 1 mother liquor water under stirring state, progressively adding weight concentration is 1 for 30-98% sulfuric acid makes aluminum ion and sulfate ion molar concentration rate: 2-2.4.
3, in meeting 2 solution, under stirring state, progressively add ammoniacal liquor or liquefied ammonia, regulate pH value, when pH value in the solution is measured as 2.5-4 with the PH1-14 test paper, stop ammonification.The better condition of pH value is 3-3.5.
4, during ammonification, temperature of charge should be less than 75 ℃.
5, under stirring state, cool off indirectly meeting 3 solution, solution temperature is dropped to below 30 ℃, obtain to contain the crystal solution of crystal;
6, emitting under the crystalline mother solution situation, crystallisate is dewatered, can adopt dehydrated forms such as vacuum, centrifugal, press filtration.
7, continue to spray crystallisate, and remove spray water, can adopt dehydrated forms such as vacuum, centrifugal, press filtration with clean water;
8, crystallisate is packed, in the plastics bag of the sealing of packing into, promptly got and pack the exsiccated ammonium alum finished product that finishes.
Produce exsiccated ammonium alum with the inventive method,, social bauxite resource is rationally utilized owing to do not use national aluminum smelting industry raw material bauxite.Present method is decomposed aluminum chloride in the Friedel-Crafts reaction and acidifying and the sulfuric acid that changes in the waste water is utilized once more.Make it to become the raw material of making exsiccated ammonium alum.Aluminium recovery can reach more than 85% in the Friedel-Crafts reaction.The sulfuric acid consumption of making exsiccated ammonium alum is than reducing 10-20% with the bauxite production method.Thereby reduced the production cost of exsiccated ammonium alum.Simultaneously, because aluminium and vitriolic are recycled, make Friedel-Crafts reaction acidifying decomposition process efflux the total amount of pollutant and reduce 50-60%; And efflux wastewater has reduced acidity PH and has been about 3.6, and waste water is more easily handled.Help environment protection.
Embodiment:
In example 1, benzene diformazan acid anhydride, the synthetic anthraquinone process of benzene production, at first use the Friedel-Crafts reaction principle, make catalyzer, make it to take place acylation reaction, under sulfuric acid and water effect, decompose then, from material, slough aluminum chloride with aluminum chloride.Get its decomposition nut liquid water 100ml, C
+++
BAL1.15mol/L, stir adding 98% sulfuric acid down, C
BSO4=2.33mol/L is under temperature of reaction 40-72 ℃ situation, with concentration 18% strong aqua conditioned reaction thing PH to 3, progressively be cooled to 25 ℃ then, separate out crystal, and carry out vacuum filtration, carry out the clean water washing to leaching crystal, obtain ammonium aluminum sulfate crystal 44.5 grams after draining.
Example 2, produce in the BB acid process, at first use Friedel-Crafts reaction, make catalyzer, make it to take place acylation reaction, under sulfuric acid and water effect, decompose then, from material, slough aluminum chloride with aluminum chloride with benzene diformazan acid anhydride, benzene.Get its decomposition nut liquid water 100ml, be concentrated to 50ml, C
+++
BAL2.31mol/L stirring down, adding 30%(weighs) sulfuric acid, C
BSO4Concentration is 2.3%mol/L, is under the 30-60 ℃ of situation in temperature of reaction, and is heavy with concentration 20%() ammoniacal liquor conditioned reaction thing pH value is 3.1, be cooled to 28 ℃ more gradually, separate out crystal, and carry out vacuum filtration, wash with clean water leaching crystal, obtain exsiccated ammonium alum 49 grams after draining.
Example 3, produce in the 2-chloroanthraquinone process, at first use Friedel-Crafts reaction, make catalyzer, make it to take place acylation reaction with aluminum chloride with chlorobenzene and benzene diformazan acid anhydride.Under sulfuric acid and water effect, decompose then, from material, slough aluminum chloride.Get its decomposition nut liquid water 100ml, C
BAL=1.31.mol/L, stirring down, adding concentration 30%(weighs) sulfuric acid, C
BSO4Be 1.7mol/L, heavy with 25%(again) ammoniacal liquor conditioned reaction thing pH value to 3, be cooled to 23 ℃ again, separate out crystal.Carry out vacuum filtration then, continue to drain with the clean water washing, get exsiccated ammonium alum 49.82 grams leaching crystal.
Above-mentioned crystallisate is tested after drying, and exsiccated ammonium alum content is all greater than the 99.5%(butt).
Claims (4)
1, a kind of method for preparing exsiccated ammonium alum, feature of the present invention is to utilize aluminium wastewater, finally by sulfuric acid, water institute's hydrolysis and change aluminium and the sulfuric acid in (mother liquor water) in the waste water over to prepares exsiccated ammonium alum with ammonia react.
2, the method for preparing exsiccated ammonium alum according to claim 1 is characterized in that described aluminium wastewater is a catalyst system therefor aluminium trichloride waste water in friedel-crafts (Friedel-Crafts) reaction.
3, according to claim 1, the 2 described methods that prepare exsiccated ammonium alum, it is characterized in that:
(1) from contain aluminum ions decomposition nut liquid water, isolate the organism of carrying secretly,
(2) make that aluminium ion concentration reaches 0.8-2.5mol/L in the mother liquor water;
(3) under stirring state, adding concentration in the mother liquor water that meets (2) is the sulfuric acid of 30%-98%, and making aluminum ion and sulfate ion molar concentration rate is 1: 2-2.4;
(4) under stirring state, in solution, add ammonia, the ammonia residual size is by the control of reaction solution pH value, and pH value is 2.5-4;
(5) temperature of charge should be less than 75 ℃ during ammonification;
(6) reactant cooling, the exsiccated ammonium alum crystallization is separated out;
(7) ammonium aluminum sulfate crystal is separated from solution;
(8) remove crystal surface impurity with clean water;
(9) exsiccated ammonium alum is divided in the packing bag.
4, the method for preparing exsiccated ammonium alum according to claim 3 is characterized in that adding ammonia in solution, and the control pH value is 3-3.5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89109109 CN1019096B (en) | 1989-12-05 | 1989-12-05 | Ammonium aluminium sulfate prodn. process from wastewater containing aluminium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89109109 CN1019096B (en) | 1989-12-05 | 1989-12-05 | Ammonium aluminium sulfate prodn. process from wastewater containing aluminium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1052291A true CN1052291A (en) | 1991-06-19 |
| CN1019096B CN1019096B (en) | 1992-11-18 |
Family
ID=4857872
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 89109109 Expired CN1019096B (en) | 1989-12-05 | 1989-12-05 | Ammonium aluminium sulfate prodn. process from wastewater containing aluminium |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1019096B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101497455A (en) * | 2009-03-13 | 2009-08-05 | 李睿德 | Method for producing limestone powder and aluminium ammonium sulfate using heat-engine plant desulfurized gypsum and fly ash |
| CN101186282B (en) * | 2007-11-23 | 2011-05-18 | 浙江苏泊尔股份有限公司 | Method for reclaiming waste sulfuric acid in hard anode oxidation process |
| CN104355374A (en) * | 2014-09-29 | 2015-02-18 | 昆明理工大学 | Sodium arsenic alunite solid solution and preparation method thereof and application of preparation method |
| CN106277010A (en) * | 2016-08-24 | 2017-01-04 | 淄博市淄川程鹏化工厂 | A kind of Alumen production technology |
| CN108328638A (en) * | 2018-03-26 | 2018-07-27 | 武汉理工大学 | A method of preparing alum from FCC dead catalyst |
-
1989
- 1989-12-05 CN CN 89109109 patent/CN1019096B/en not_active Expired
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101186282B (en) * | 2007-11-23 | 2011-05-18 | 浙江苏泊尔股份有限公司 | Method for reclaiming waste sulfuric acid in hard anode oxidation process |
| CN101497455A (en) * | 2009-03-13 | 2009-08-05 | 李睿德 | Method for producing limestone powder and aluminium ammonium sulfate using heat-engine plant desulfurized gypsum and fly ash |
| CN101497455B (en) * | 2009-03-13 | 2014-03-05 | 李睿德 | Method for producing limestone powder and aluminium ammonium sulfate using heat-engine plant desulfurized gypsum and fly ash |
| CN104355374A (en) * | 2014-09-29 | 2015-02-18 | 昆明理工大学 | Sodium arsenic alunite solid solution and preparation method thereof and application of preparation method |
| CN106277010A (en) * | 2016-08-24 | 2017-01-04 | 淄博市淄川程鹏化工厂 | A kind of Alumen production technology |
| CN108328638A (en) * | 2018-03-26 | 2018-07-27 | 武汉理工大学 | A method of preparing alum from FCC dead catalyst |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1019096B (en) | 1992-11-18 |
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