CN102180500A - Method for preparing aluminium nitrate and ferric nitrate high hydrates combined with potassium nitrate and calcium sulfate by alum sludge - Google Patents

Method for preparing aluminium nitrate and ferric nitrate high hydrates combined with potassium nitrate and calcium sulfate by alum sludge Download PDF

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CN102180500A
CN102180500A CN2010105666237A CN201010566623A CN102180500A CN 102180500 A CN102180500 A CN 102180500A CN 2010105666237 A CN2010105666237 A CN 2010105666237A CN 201010566623 A CN201010566623 A CN 201010566623A CN 102180500 A CN102180500 A CN 102180500A
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nitrate
water
calcium sulfate
nitrates
saltpetre
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王嘉兴
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汪晋强
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Abstract

The invention provides a method for aluminium nitrate and ferric nitrate high hydrates combined with potassium nitrate and calcium sulfate by alum sludge; alum sludge is fully dissolved in water and filtered, and the filtrate is a mixture of potassium sulfate, aluminum sulfate and ferric sulfate; the filtrate is allowed to react with calcium nitrate to obtain a mixture of calcium sulfate precipitates, aluminium nitrate nonahydrate, ferric nitrate nonahydrate and potassium nitrate solutions, and the mixture is filtered to obtain calcium sulfate precipitates and a filtrate of aluminium nitrate nonahydrate, ferric nitrate nonahydrate and potassium nitrate; the filtrate is distilled at a reduced pressure, and because of the different freezing points of aluminium nitrate nonahydrate, ferric nitrate nonahydrate and potassium nitrate, the saturated solution is cooled gradually from a high temperature to a low temperature so as to perform crystallization and to precipitate aluminium nitrate nonahydrate, ferric nitrate nonahydrate and potassium nitrate in turn; the precipitates are filtered and dried to obtain an aluminium nitrate nonahydrate product, a ferric nitrate nonahydrate product and a potassium nitrate product respectively. The method prepares aluminium nitrate and ferric nitrate high hydrates combined with potassium nitrate and calcium sulfate products by alum sludge through simple processing, makes full use of the potential value of alum sludge, does not produce secondary pollution, and is an economical and applicable method with the capability to change waste into valuables.

Description

The method for preparing aluminum nitrate and the high water thing of iron nitrate coproduction saltpetre and calcium sulfate with the alum slurry
Technical field
The present invention relates to inorganic chemical industry three wastes alum slurry and administer and utilize technical field, especially prepare the method for aluminum nitrate and the high water thing of iron nitrate coproduction saltpetre and calcium sulfate with the alum slurry.
Background technology
Alum claims potassium aluminium alum again, and arcanite and potassium alum, chemical formula are K 2SO 4Al 2(SO 4) 324H 2O or KAl (SO 4) 224H 2O is the double salt that contains the aluminum potassium sulfate of crystal water, and is soluble in water, hydrolysis takes place when water-soluble and generates the gluey precipitation of aluminium hydroxide, loses crystal water when being heated and forms white powder and be called for short exsiccated alum.
Alum is widely used in industries such as chemical industry, food, daily use chemicals, water treatment, and its consumption is very huge.Its main production raw material is an alunite, mainly is distributed in provinces such as China Zhejiang, Anhui, and production method mainly contains pickling process, ammonia leaching process, water seaoning, reduction heat solution.No matter which kind of mode to produce alum, all can produce a large amount of high alumina alum slurries with.Owing to contain impurity such as a large amount of silicon, iron simultaneously in the alum slurry, air storage throughout the year not only makes mentioned component be difficult to development and use, also can cause sour water to run off contaminate environment.
Though at present also there are some further investigations to the alunite comprehensive utilization in China, have developed and utilized alunite to produce gained alum slurry manufacture sylvite behind the alum, aluminum oxide series raw material, various aluminium salt etc.The appearance of above-mentioned technology is for comprehensive utilization alum slurry has been opened up market.Yet the industrial utilization of alum slurry does not still have sophisticated example so far at home and abroad.Especially, a lot of technologies have occurred the phenomenon of secondary pollution again in improvement and utilization processing to the alum slurry.
Therefore, be necessary to explore new alum slurry improvement and utilize method, make full use of the potential value of alum slurry, develop useful product.
Summary of the invention
The objective of the invention is to, a kind of method for preparing aluminum nitrate and the high water thing of iron nitrate coproduction saltpetre and calcium sulfate with the alum slurry is provided, this method is produced the waste material alum slurry of gained behind the alum with alunite, through simple processing treatment, make the high water thing of aluminum nitrate and iron nitrate coproduction saltpetre and calcium sulfate, made full use of the potential value of alum slurry, and do not produced secondary pollution, being one turns waste into wealth, economic and practical method.
Technical scheme of the present invention is as follows: a kind ofly prepare the method for aluminum nitrate and the high water thing of iron nitrate coproduction saltpetre and calcium sulfate with alum slurry, comprise following concrete steps:
Steps A, with the alum slurry retort one (1) of packing into, the abundant stirring made it to be dissolved in water in 0.5-2 hour after adding water, then passed through filter one (2) and filtered, and obtained filter cake and filtrate, filter cake is through other technology deep processing, and filtrate is the mixture of vitriolate of tartar and Tai-Ace S 150 and ferric sulfate;
Step B, steps A gained filtrate is sent into retort two (3), ratio according to Tai-Ace S 150 and nitrocalcite pure substance quality is 1: 3.84-5.00 throws ca nitrate soln in retort two (3), and reaction obtains the mixture of calcium sulfate precipitation, nine water aluminum nitrates, nine water iron nitrates, potassium nitrate solution under the stirring that blows slowly;
Step C, step B gained mixture is filtered through filter two (4), obtain calcium sulfate precipitation and contain the solution of nine water aluminum nitrates, nine water iron nitrates, saltpetre; Calcium sulfate precipitation is through washing machine (5) washing, moisture eliminator (6) drying, and pulverizer (7) is pulverized, and obtains calcium sulfate product (12);
Step D, the solution that contains nine water aluminum nitrates, nine water iron nitrates, saltpetre are sent into underpressure distillation in the underpressure distillation device (8), when solution distills saturated solution, zero pour difference according to nine water aluminum nitrates, nine water iron nitrates, saltpetre, temperature cooling gradually from high to low with saturated solution, nine water iron nitrates, nine water aluminum nitrates, saltpetre crystallization are successively separated out, and filtration drying obtains nine water iron nitrate products (9) respectively, nine water aluminum nitrate products (10), saltpetre product (11).
Of the present inventionly prepare the method for aluminum nitrate and the high water thing of iron nitrate coproduction saltpetre and calcium sulfate with alum slurry, chemical principle is:
SO 3+H 2O====H 2SO 4
Al 2O 3+3H 2SO 4=====Al 2(SO 4) 3+3H 2O
K 2O+H 2SO 4=====K 2SO 4+H 2O
Fe 2O 3+3H 2SO 4=====Fe 2(SO 4) 3+3H 2O
Al 2(SO 4) 3+3Ca(NO 3) 2+9H 2O=====2Al(NO 3) 3·9H 2O+3CaSO 4
Fe 2(SO 4)+3Ca(NO 3) 2+9H 2O=====2Fe(NO 3) 3·9H 2O+3CaSO 4
K 2SO 4+Ca(NO 3) 2=====2KNO 3+CaSO 4
Beneficial effect of the present invention is: the method for preparing aluminum nitrate and the high water thing of iron nitrate coproduction saltpetre and calcium sulfate with the alum slurry of the present invention, waste material alum slurry with gained behind the alunite production alum, through simple processing treatment, make the high water thing of aluminum nitrate and iron nitrate coproduction saltpetre and calcium sulfate, made full use of the potential value of alum slurry, and do not produce secondary pollution, being one turns waste into wealth, economic and practical method.This method is simple to operate, and facility investment is few, is worthy of popularization.
Description of drawings
Fig. 1 of the present inventionly prepares the process flow sheet of the method for aluminum nitrate and the high water thing of iron nitrate coproduction saltpetre and calcium sulfate with alum slurry, wherein, and (1) retort one, (2) strainer one, retort two (3), (4) strainer two, (5) washing machine, (6) moisture eliminator, (7) pulverizer, (8) underpressure distillation device, (9) nine water iron nitrate products, (10) nine water aluminum nitrate products, (11) potassium product, (12) calcium sulfate product.
Embodiment
Embodiment 1:
With reference to Fig. 1, a kind of method for preparing aluminum nitrate and the high water thing of iron nitrate coproduction saltpetre and calcium sulfate with the alum slurry, alum is starched the retort one (1) of packing into, the abundant stirring made it to be dissolved in water in 0.5-2 hour after adding water, then passing through filter one (2) filters, obtain filter cake and filtrate, filter cake is through other technology deep processing, and filtrate is the mixture of vitriolate of tartar and Tai-Ace S 150 and ferric sulfate; Gained filtrate is sent into retort two (3), and the quality that makes ferric sulfate in the retort is 400kg, the quality of Tai-Ace S 150 is 171kg, the quality of vitriolate of tartar is 87kg, according to the ratio of Tai-Ace S 150 and nitrocalcite pure substance quality is to retort two (3) in to throw ca nitrate soln at 1: 4.80, and reaction obtains the mixture of calcium sulfate precipitation, nine water aluminum nitrates, nine water iron nitrates, potassium nitrate solution under the stirring that blows slowly; The gained mixture is filtered through filter two (4), obtain calcium sulfate precipitation and the solution that contains nine water aluminum nitrates, nine water iron nitrates, saltpetre; Calcium sulfate precipitation is through washing machine (5) washing, moisture eliminator (6) drying, and pulverizer (7) is pulverized, and obtains calcium sulfate product (12); The solution that will contain nine water aluminum nitrates, nine water iron nitrates, saltpetre is sent into underpressure distillation in the underpressure distillation device (8), when solution distills saturated solution, zero pour difference according to nine water aluminum nitrates, nine water iron nitrates, saltpetre, temperature cooling gradually from high to low with saturated solution, nine water iron nitrates, nine water aluminum nitrates, saltpetre crystallization are successively separated out, and filtration drying obtains nine water iron nitrate products (9) respectively, nine water aluminum nitrate products (10), potassium product (11).
Wherein the lime carbonate that contains of calcium sulfate product is 680kg, and the nine water iron nitrates that nine water iron nitrate products contain are 808kg, and the nine water aluminum nitrates that nine water aluminum nitrate products contain are 375kg, and the saltpetre that potassium product contains is 101kg.
Embodiment 2:
With reference to Fig. 1, a kind of method for preparing aluminum nitrate and the high water thing of iron nitrate coproduction saltpetre and calcium sulfate with the alum slurry, alum is starched the retort one (1) of packing into, the abundant stirring made it to be dissolved in water in 0.5-2 hour after adding water, then passing through filter one (2) filters, obtain filter cake and filtrate, filter cake is through other technology deep processing, and filtrate is the mixture of vitriolate of tartar and Tai-Ace S 150 and ferric sulfate; Gained filtrate is sent into retort two (3), and the quality that makes ferric sulfate in the retort is 400kg, the quality of Tai-Ace S 150 is 171kg, the quality of vitriolate of tartar is 87kg, according to the ratio of Tai-Ace S 150 and nitrocalcite pure substance quality is to retort two (3) in to throw ca nitrate soln at 1: 5.00, and reaction obtains the mixture of calcium sulfate precipitation, nine water aluminum nitrates, nine water iron nitrates, potassium nitrate solution under the stirring that blows slowly; The gained mixture is filtered through filter two (4), obtain calcium sulfate precipitation and the solution that contains nine water aluminum nitrates, nine water iron nitrates, saltpetre; Calcium sulfate precipitation is through washing machine (5) washing, moisture eliminator (6) drying, and pulverizer (7) is pulverized, and obtains calcium sulfate product (12); The solution that will contain nine water aluminum nitrates, nine water iron nitrates, saltpetre is sent into underpressure distillation in the underpressure distillation device (8), when solution distills saturated solution, zero pour difference according to nine water aluminum nitrates, nine water iron nitrates, saltpetre, temperature cooling gradually from high to low with saturated solution, nine water iron nitrates, nine water aluminum nitrates, saltpetre crystallization are successively separated out, and filtration drying obtains nine water iron nitrate products (9) respectively, nine water aluminum nitrate products (10), saltpetre product (11).
Wherein the lime carbonate that contains of calcium sulfate product is 680kg, and the nine water iron nitrates that nine water iron nitrate products contain are 808kg, and the nine water aluminum nitrates that nine water aluminum nitrate products contain are 375kg, and the saltpetre that potassium product contains is 101kg.
Embodiment 3:
With reference to Fig. 1, a kind of method for preparing aluminum nitrate and the high water thing of iron nitrate coproduction saltpetre and calcium sulfate with the alum slurry, alum is starched the retort one (1) of packing into, the abundant stirring made it to be dissolved in water in 0.5-2 hour after adding water, then passing through filter one (2) filters, obtain filter cake and filtrate, filter cake is through other technology deep processing, and filtrate is the mixture of vitriolate of tartar and Tai-Ace S 150 and ferric sulfate; Gained filtrate is sent into retort two (3), and the quality that makes ferric sulfate in the retort is 400kg, the quality of Tai-Ace S 150 is 171kg, the quality of vitriolate of tartar is 87kg, according to the ratio of Tai-Ace S 150 and nitrocalcite pure substance quality is to retort two (3) in to throw ca nitrate soln at 1: 3.84, and reaction obtains the mixture of calcium sulfate precipitation, nine water aluminum nitrates, nine water iron nitrates, potassium nitrate solution under the stirring that blows slowly; The gained mixture is filtered through filter two (4), obtain calcium sulfate precipitation and the solution that contains nine water aluminum nitrates, nine water iron nitrates, saltpetre; Calcium sulfate precipitation is through washing machine (5) washing, moisture eliminator (6) drying, and pulverizer (7) is pulverized, and obtains calcium sulfate product (12); The solution that will contain nine water aluminum nitrates, nine water iron nitrates, saltpetre is sent into underpressure distillation in the underpressure distillation device (8), when solution distills saturated solution, zero pour difference according to nine water aluminum nitrates, nine water iron nitrates, saltpetre, temperature cooling gradually from high to low with saturated solution, nine water iron nitrates, nine water aluminum nitrates, vitriolate of tartar crystallization are successively separated out, and filtration drying obtains nine water iron nitrate products (9) respectively, nine water aluminum nitrate products (10), potassium product (11).
Wherein the lime carbonate that contains of calcium sulfate product is 544kg, and the nine water iron nitrates that nine water iron nitrate products contain are 646.4kg, and the nine water aluminum nitrates that nine water aluminum nitrate products contain are 300kg, and the saltpetre that potassium product contains is 80.8kg.
Above content be in conjunction with concrete preferred implementation to further describing that the present invention did, can not assert that concrete enforcement of the present invention is confined to these explanations.For the general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, its framework form can be flexible and changeable, can the subseries product.Just make some simple deduction or replace, all should be considered as belonging to the scope of patent protection that the present invention is determined by claims of being submitted to.

Claims (1)

1. one kind prepares the method for aluminum nitrate and the high water thing of iron nitrate coproduction saltpetre and calcium sulfate with alum slurry, comprises following concrete steps:
Steps A, with the alum slurry retort one (1) of packing into, the abundant stirring made it to be dissolved in water in 0.5-2 hour after adding water, then passed through filter one (2) and filtered, and obtained filter cake and filtrate, filter cake is through other technology deep processing, and filtrate is the mixture of vitriolate of tartar and Tai-Ace S 150 and ferric sulfate;
Step B, steps A gained filtrate is sent into retort two (3), ratio according to Tai-Ace S 150 and nitrocalcite pure substance quality is 1: 3.84-5.00 throws ca nitrate soln in retort two (3), and reaction obtains the mixture of calcium sulfate precipitation, nine water aluminum nitrates, nine water iron nitrates, potassium nitrate solution under the stirring that blows slowly;
Step C, step B gained mixture is filtered through filter two (4), obtain calcium sulfate precipitation and contain the solution of nine water aluminum nitrates, nine water iron nitrates, saltpetre; Calcium sulfate precipitation is through washing machine (5) washing, moisture eliminator (6) drying, and pulverizer (7) is pulverized, and obtains calcium sulfate product (12);
Step D, the solution that contains nine water aluminum nitrates, nine water iron nitrates, saltpetre are sent into underpressure distillation in the underpressure distillation device (8), when solution distills saturated solution, zero pour difference according to nine water aluminum nitrates, nine water iron nitrates, saltpetre, temperature cooling gradually from high to low with saturated solution, nine water iron nitrates, nine water aluminum nitrates, saltpetre crystallization are successively separated out, and filtration drying obtains nine water iron nitrate products (9) respectively, nine water aluminum nitrate products (10), saltpetre product (11).
CN2010105666237A 2010-11-30 2010-11-30 Method for preparing aluminium nitrate and ferric nitrate high hydrates combined with potassium nitrate and calcium sulfate by alum sludge Pending CN102180500A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106629805A (en) * 2016-10-17 2017-05-10 交城县三喜化工有限公司 Method and device for producing calcium nitrate liquid

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106629805A (en) * 2016-10-17 2017-05-10 交城县三喜化工有限公司 Method and device for producing calcium nitrate liquid
CN106629805B (en) * 2016-10-17 2017-11-21 交城县三喜化工有限公司 A kind of method and its device for producing calcium nitrate liquid

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Application publication date: 20110914