CN102249314A - Method for preparing chromic hydroxide, lead chloride and sodium nitrate by chromium-containing mirabilite - Google Patents
Method for preparing chromic hydroxide, lead chloride and sodium nitrate by chromium-containing mirabilite Download PDFInfo
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- CN102249314A CN102249314A CN2010105980169A CN201010598016A CN102249314A CN 102249314 A CN102249314 A CN 102249314A CN 2010105980169 A CN2010105980169 A CN 2010105980169A CN 201010598016 A CN201010598016 A CN 201010598016A CN 102249314 A CN102249314 A CN 102249314A
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- chromium
- chloride
- filter cake
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
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Abstract
The invention provides a method for preparing chromic hydroxide, lead chloride and sodium nitrate by chromium-containing mirabilite. The chromium-containing mirabilite is mixed with hydrochloric acid for reacting to obtain a mixture containing chromic chloride, sodium chloride and nitric acid; mixed liquor and a filter cake containing silicon dioxide are obtained by extraction filtration; the obtained mixed liquor and excess industrial water are mixed to hydrolyze the chromic chloride into trivalent chromium chromic hydroxide which is settled; a clear mixed liquid containing the sodium chloride and the nitric acid and a chromic hydroxide filter cake are obtained by extraction filtration; the chromic hydroxide filter cake is washed, dried and smashed to obtain the chromic hydroxide product; the clear mixed liquid containing the sodium chloride and the nitric acid reacts with lead chloride to remove impurities by filtering to obtain a clear filtrate and a lead chloride filter cake; the clear filtrate is cooled and crystallized after reduced pressure distillation to separate out sodium chloride crystals; a sodium chloride product is obtained by rectification; and the lead nitrate filter cake is washed, dried and smashed to obtain the lead nitrate product.
Description
Technical field
The present invention relates to the improvement of inorganic chemical industry three wastes chromium slag and utilize technical field, relate in particular to a kind of usefulness and contain the method that the chromium saltcake prepares chromium hydroxide, lead chloride and SODIUMNITRATE.
Background technology
The chromium slag is meant that in the sodium dichromate 99 production process chromite is through using the residue of water extraction sodium dichromate 99 after the roasting.Because raw materials used, production technique and prescription are different, the chromium slag is formed different, the composition that it is basic and the per-cent of composition are as follows: the chromium sesquioxide mass percent is 2.5-4%, water-soluble sexavalent chrome mass percent is 0.28-1.34%, and solubility in acid sexavalent chrome mass percent is 0.9-1.4﹠amp; , the calcium oxide mass percent is 29-36﹠amp; , magnesium oxide quality percentage ratio 20-33%, the aluminium sesquioxide mass percent is 5-8%, silicon-dioxide quality percentage ratio is 8-11%.Because the sexavalent chrome that contains in the chromium slag has strong oxidizing property, organism is caused intensive corrosion and destroys, and in a single day soil and underground water are subjected to chromic pollution, and soil can not farming, underground water can't be drunk, thereby is the carcinogenic substance and the hypertoxicity thing of MA.Therefore,, separate the toxicity of dechromisation slag if can not take special control measures that the chromium slag is handled, in case polluted environment, particularly underground water and soil, its consequence is very serious.
In addition, also contain a large amount of useful compositions in the chromium slag, be necessary it is purified and conversion process, to give full play to the economic worth of chromium slag.
Summary of the invention
The objective of the invention is to, provide a kind of usefulness to contain the method that the chromium saltcake prepares chromium hydroxide, lead chloride and SODIUMNITRATE, this method will contain the chromium saltcake through simple processing treatment, make original deleterious sexavalent chrome, become nontoxic trivalent chromium, make chromium hydroxide and lead chloride and SODIUMNITRATE, the potential value that contains the chromium saltcake that has made full use of, and do not produce secondary pollution, being one turns waste into wealth, economic and practical method.
Technical scheme of the present invention is as follows: a kind of usefulness contains the method that the chromium saltcake prepares chromium hydroxide, lead chloride and SODIUMNITRATE, comprises following concrete steps:
Steps A: the ratio by the molar content of the material of the hydrogenchloride that contains in the molar content sum that contains the chromium trioxide that contains in the chromium saltcake and SODIUMNITRATE and the hydrochloric acid is 1: 0.8-1.2 will contain the chromium saltcake and hydrochloric acid drops into hybrid reaction in the corrosion-resistant reactor one (1), obtain containing the mixture of chromium chloride, sodium-chlor and nitric acid, reactant obtains mixed solution and silica containing filter cake through suction filtration machine one (2) suction filtration;
Step B: steps A gained mixed solution is sent into slurry tank (3) lining, and add excessive service water, make the chromium chloride hydrolysis form the trivalent chromium chromium hydroxide and sedimentation, obtain sodium chloride-containing and nitric acid clarification mixed solution and chromium hydroxide filter cake through suction filtration machine two (4) suction filtrations again;
Step C: chromium hydroxide product (8) is pulverized, obtained to the chromium hydroxide filter cake through washing machine one (5), drying machine one (6) drying, pulverizer one (7);
Step D: sodium chloride-containing and nitric acid clarification mixed solution are sent in the corrosion-resistant reactor two (9), ratio according to nitric acid and the molar content of the pure substance of lead chloride is 1: 0.4-0.6 drops into lead chloride solution, obtain containing the solution of lead nitrate, hydrogenchloride and sodium-chlor, filter through filter (10), obtain lead nitrate filter cake and clarifying filtrate;
Step e: the clarifying filtrate of step D gained is sent in the underpressure distillation device (11), the decompression intensification reaches the evaporation of water point and evaporates the water, become sodium chloride saturated solution and then enter cooling crystallizer (12) lining crystallisation by cooling, the precipitated sodium chloride crystal obtains sodium-chlor product (13) by rectifying again; Residual solution is that hydrochloric acid soln returns the steps A recycle;
Step F: lead nitrate product (17) is pulverized, obtained to gained lead nitrate filter cake through washing machine two (14), drying machine two (15) dryings, pulverizer two (16).
It should be noted that in the steps A can not add excessive service water in the corrosion-resistant reactor,, mix in the remaining residue in order to avoid cause the chromium chloride premature hydrolysis to form chromic chromium hydroxide.
Usefulness of the present invention contains the method that the chromium saltcake prepares chromium hydroxide, lead chloride and SODIUMNITRATE, and its chemical principle is:
2CrO
3+12HCl=====2CrCl
3+3Cl
2+6H
2O
CrCl
3+3H
2O=====Cr(OH)
3+3HCl
NaNO
3+HCl=====NaCl+HNO
3
2HNO
3+PbCl
2=====Pb(NO
3)
2+2HCl
Beneficial effect of the present invention is: usefulness of the present invention contains the method that the chromium saltcake prepares chromium hydroxide, lead chloride and SODIUMNITRATE, through simple processing treatment, make chromium hydroxide and lead chloride and SODIUMNITRATE, made full use of the potential value that contains the chromium saltcake, 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 contains the process flow sheet that the chromium saltcake prepares the method for chromium hydroxide, lead chloride and SODIUMNITRATE for usefulness of the present invention, wherein, (1) corrosion-resistant reactor one, (2) the suction filtration machine one, (3) in the slurry tank, (4) the suction filtration machine two, (5) washing machine one, (6) drying machine one, (7) pulverizer one, (8) corrosion-resistant reactor two, (9) chromium hydroxide product, (10) strainer, (11) underpressure distillation device, (12) cooling crystallizer, (13) sodium-chlor product, (14) washing machine two, (15) drying machine two, (16) pulverizer two, (17) lead nitrate product.
Embodiment
Embodiment 1:
With reference to Fig. 1, a kind of usefulness contains the method that the chromium saltcake prepares chromium hydroxide, lead chloride and SODIUMNITRATE, comprises following concrete steps:
Steps A: take by weighing contain 200 chromium trioxides and 380kg SODIUMNITRATE contain the chromium saltcake, by the ratio of the molar content of the material of the hydrogenchloride that contains in the molar content sum that contains the chromium trioxide that contains in the chromium saltcake and SODIUMNITRATE and the hydrochloric acid is will contain chromium saltcake at 1: 0.8 and hydrochloric acid drops into hybrid reaction in the corrosion-resistant reactor one (1), obtain containing the mixture of chromium chloride, sodium-chlor and nitric acid, reactant obtains mixed solution and silica containing filter cake through suction filtration machine one (2) suction filtration;
Step B: steps A gained mixed solution is sent into slurry tank (3) lining, and add excessive service water, make the chromium chloride hydrolysis form the trivalent chromium chromium hydroxide and sedimentation, obtain sodium chloride-containing and nitric acid clarification mixed solution and chromium hydroxide filter cake through suction filtration machine two (4) suction filtrations again;
Step C: chromium hydroxide product (8) is pulverized, obtained to the chromium hydroxide filter cake through washing machine one (5), drying machine one (6) drying, pulverizer one (7), and the quality of the chromium hydroxide pure substance that it contains is 193.6kg;
Step D: sodium chloride-containing and nitric acid clarification mixed solution are sent in the corrosion-resistant reactor two (9), according to the ratio of nitric acid and the molar content of the pure substance of lead chloride is to drop into lead chloride solution at 1: 0.4, obtain containing the solution of lead nitrate, hydrogenchloride and sodium-chlor, filter through filter (10), obtain lead nitrate filter cake and clarifying filtrate;
Step e: the clarifying filtrate of step D gained is sent in the underpressure distillation device (11), the decompression intensification reaches the evaporation of water point and evaporates the water, become sodium chloride saturated solution and then enter cooling crystallizer (12) lining crystallisation by cooling, the precipitated sodium chloride crystal, obtain sodium-chlor product (13) by rectifying again, the quality of the sodium-chlor pure substance that it contains is 187.2kg; Residual solution is that hydrochloric acid soln returns the steps A recycle;
Step F: lead nitrate product (17) is pulverized, obtained to gained lead nitrate filter cake through washing machine two (14), drying machine two (15) dryings, pulverizer two (16), and the quality of the lead nitrate pure substance that it contains is 423.68kg.
Embodiment 2:
With reference to Fig. 1, a kind of usefulness contains the method that the chromium saltcake prepares chromium hydroxide, lead chloride and SODIUMNITRATE, comprises following concrete steps:
Steps A: take by weighing contain 200 chromium trioxides and 380kg SODIUMNITRATE contain the chromium saltcake, by the ratio of the molar content of the material of the hydrogenchloride that contains in the molar content sum that contains the chromium trioxide that contains in the chromium saltcake and SODIUMNITRATE and the hydrochloric acid is will contain chromium saltcake at 1: 1 and hydrochloric acid drops into hybrid reaction in the corrosion-resistant reactor one (1), obtain containing the mixture of chromium chloride, sodium-chlor and nitric acid, reactant obtains mixed solution and silica containing filter cake through suction filtration machine one (2) suction filtration;
Step B: steps A gained mixed solution is sent into slurry tank (3) lining, and add excessive service water, make the chromium chloride hydrolysis form the trivalent chromium chromium hydroxide and sedimentation, obtain sodium chloride-containing and nitric acid clarification mixed solution and chromium hydroxide filter cake through suction filtration machine two (4) suction filtrations again;
Step C: chromium hydroxide product (8) is pulverized, obtained to the chromium hydroxide filter cake through washing machine one (5), drying machine one (6) drying, pulverizer one (7), and the amount of the chromium hydroxide pure substance that it contains is 242kg;
Step D: sodium chloride-containing and nitric acid clarification mixed solution are sent in the corrosion-resistant reactor two (9), according to the ratio of nitric acid and the molar content of the pure substance of lead chloride is to drop into lead chloride solution at 1: 0.5, obtain containing the solution of lead nitrate, hydrogenchloride and sodium-chlor, filter through filter (10), obtain lead nitrate filter cake and clarifying filtrate;
Step e: the clarifying filtrate of step D gained is sent in the underpressure distillation device (11), the decompression intensification reaches the evaporation of water point and evaporates the water, become sodium chloride saturated solution and then enter cooling crystallizer (12) lining crystallisation by cooling, the precipitated sodium chloride crystal, obtain sodium-chlor product (13) by rectifying again, the quality of the sodium-chlor pure substance that it contains is 234kg; Residual solution is that hydrochloric acid soln returns the steps A recycle;
Step F: lead nitrate product (17) is pulverized, obtained to gained lead nitrate filter cake through washing machine two (14), drying machine two (15) dryings, pulverizer two (16), and the quality of the lead nitrate pure substance that it contains is 674kg.
Embodiment 3:
With reference to Fig. 1, a kind of usefulness contains the method that the chromium saltcake prepares chromium hydroxide, lead chloride and SODIUMNITRATE, comprises following concrete steps:
Steps A: take by weighing contain 200 chromium trioxides and 380kg SODIUMNITRATE contain the chromium saltcake, by the ratio of the molar content of the material of the hydrogenchloride that contains in the molar content sum that contains the chromium trioxide that contains in the chromium saltcake and SODIUMNITRATE and the hydrochloric acid is will contain chromium saltcake at 1: 1.2 and hydrochloric acid drops into hybrid reaction in the corrosion-resistant reactor one (1), obtain containing the mixture of chromium chloride, sodium-chlor and nitric acid, reactant obtains mixed solution and silica containing filter cake through suction filtration machine one (2) suction filtration;
Step B: steps A gained mixed solution is sent into slurry tank (3) lining, and add excessive service water, make the chromium chloride hydrolysis form the trivalent chromium chromium hydroxide and sedimentation, obtain sodium chloride-containing and nitric acid clarification mixed solution and chromium hydroxide filter cake through suction filtration machine two (4) suction filtrations again;
Step C: chromium hydroxide product (8) is pulverized, obtained to the chromium hydroxide filter cake through washing machine one (5), drying machine one (6) drying, pulverizer one (7), and the amount of the chromium hydroxide pure substance that it contains is 242kg;
Step D: sodium chloride-containing and nitric acid clarification mixed solution are sent in the corrosion-resistant reactor (9), according to the ratio of nitric acid and the molar content of the pure substance of lead chloride is to drop into lead chloride solution at 1: 0.6, obtain containing the solution of lead nitrate, hydrogenchloride and sodium-chlor, filter through filter (10), obtain lead nitrate filter cake and clarifying filtrate;
Step e: the clarifying filtrate of step D gained is sent in the underpressure distillation device (11), the decompression intensification reaches the evaporation of water point and evaporates the water, become sodium chloride saturated solution and then enter cooling crystallizer (12) lining crystallisation by cooling, the precipitated sodium chloride crystal, obtain sodium-chlor product (13) by rectifying again, the quality of the sodium-chlor pure substance that it contains is 234kg; Residual solution is that hydrochloric acid soln returns the steps A recycle;
Step F: lead nitrate product (17) is pulverized, obtained to gained lead nitrate filter cake through washing machine two (14), drying machine two (15) dryings, pulverizer two (16), and the quality of the lead nitrate pure substance that it contains is 674kg.
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 with containing the method that the chromium saltcake prepares chromium hydroxide, lead chloride and SODIUMNITRATE, it is characterized in that, comprises following concrete steps:
Steps A: the ratio by the molar content of the material of the hydrogenchloride that contains in the molar content sum that contains the chromium trioxide that contains in the chromium saltcake and SODIUMNITRATE and the hydrochloric acid is 1: 0.8-1.2 will contain the chromium saltcake and hydrochloric acid drops into hybrid reaction in the corrosion-resistant reactor one (1), obtain containing the mixture of chromium chloride, sodium-chlor and nitric acid, reactant obtains mixed solution and silica containing filter cake through suction filtration machine one (2) suction filtration;
Step B: steps A gained mixed solution is sent into slurry tank (3) lining, and add excessive service water, make the chromium chloride hydrolysis form the trivalent chromium chromium hydroxide and sedimentation, obtain sodium chloride-containing and nitric acid clarification mixed solution and chromium hydroxide filter cake through suction filtration machine two (4) suction filtrations again;
Step C: chromium hydroxide product (8) is pulverized, obtained to the chromium hydroxide filter cake through washing machine one (5), drying machine one (6) drying, pulverizer one (7);
Step D: sodium chloride-containing and nitric acid clarification mixed solution are sent in the corrosion-resistant reactor two (9), ratio according to nitric acid and the molar content of the pure substance of lead chloride is 1: 0.4-0.6 drops into lead chloride solution, obtain containing the solution of lead nitrate, hydrogenchloride and sodium-chlor, filter through filter (10), obtain lead nitrate filter cake and clarifying filtrate;
Step e: the clarifying filtrate of step D gained is sent in the underpressure distillation device (11), the decompression intensification reaches the evaporation of water point and evaporates the water, become sodium chloride saturated solution and then enter cooling crystallizer (12) lining crystallisation by cooling, the precipitated sodium chloride crystal obtains sodium-chlor product (13) by rectifying again; Residual solution is that hydrochloric acid soln returns the steps A recycle;
Step F: lead nitrate product (17) is pulverized, obtained to gained lead nitrate filter cake through washing machine two (14), drying machine two (15) dryings, pulverizer two (16).
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Cited By (1)
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CN110817960A (en) * | 2019-12-26 | 2020-02-21 | 四川省银河化学股份有限公司 | Method for preparing chromium chloride hexahydrate by using sodium chromate |
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CN110817960A (en) * | 2019-12-26 | 2020-02-21 | 四川省银河化学股份有限公司 | Method for preparing chromium chloride hexahydrate by using sodium chromate |
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Application publication date: 20111123 |