CN101955195A - Method for preparing zinc cyanide and jointly producing mixed sulfates from waste residues in Sodamide method - Google Patents

Method for preparing zinc cyanide and jointly producing mixed sulfates from waste residues in Sodamide method Download PDF

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Publication number
CN101955195A
CN101955195A CN 201010190357 CN201010190357A CN101955195A CN 101955195 A CN101955195 A CN 101955195A CN 201010190357 CN201010190357 CN 201010190357 CN 201010190357 A CN201010190357 A CN 201010190357A CN 101955195 A CN101955195 A CN 101955195A
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waste residue
zinc cyanide
temperature
sodium
sodamide
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CN 201010190357
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Chinese (zh)
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王嘉兴
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汪晋强
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Abstract

The invention relates to the technical field of comprehensive treatment and utilization of waste residues in a Sodamide method, in particular to a method for preparing zinc cyanide and jointly producing mixed sulfates from the waste residue in the Sodamide method. The method has the main technical scheme that the method includes the following steps of: firstly, placing the waste residues in the sodamide method and sodium sulfate according to the pure substance mass ratio of 1:(1.18-1.58) in a low-temperature closed reaction kettle for reaction, filtering after reaction, and burning filter cake impurities; firstly distilling the filtrate at low temperature in a reduced pressure distiller, and then crystallizing in a low-temperature crystallizer; and finally, preparing zinc cyanide crystals and the mixed sulfates. The invention not only has simple and feasible preparation process and equipment, but also has low cost; particularly, the invention can thoroughly remove CN- in the waste residues so as to eliminate influence on environment, and meanwhile, products with certain economical value can be created.

Description

Ammonia sodium method waste residue prepares the method for zinc cyanide coproduction mixed sulfate
Technical field
The present invention relates to the technical field of the comprehensive regulation of prussiate waste residue and utilization, especially prepare the method for zinc cyanide coproduction mixed sulfate with ammonia sodium method waste residue.
Technical background
Ammonia sodium method is to be raw material with charcoal, sodium Metal 99.5, liquefied ammonia mainly, the method of in reactor, directly synthesizing sodium cyanide, containing the cyanogen amount in the slag that is produced in its preparation process is 1~4%, prussiate is because it has toxicity, its manufacturing enterprise belongs to the object of state key environmental protection and improvement, its all strict control of each program and protection are that the master gas or the outdoor air index in workshop all is strict the detection, and are controlled.The discharging of the three wastes is added on tight especially tight, so on the dynamics of administering careful usually degree to the cyanogen molecular diffusion.Prussiate is produced the hydrogen cyanogen root in the waste residue because severe toxicity is arranged, if washing does not totally not only have very big pollution to environment, by biological cycle, also there is very big potentially dangerous in the people; And because the amount of waste residue is big, stacking also can take and corrode a large amount of limited land resources.For containing the cyanogen material no matter be reasonably to emit after gas, liquid or solid the like waste all will decompose and administer." industry " three wastes " discharging tentative standard " is 0.5mg/L (in free cyanogen root) to the highest permission emission concentration of prussiate in the trade effluent (GBJ4-73).
Chinese patent, application number is 200510056582, denomination of invention is the method for desuifurized system gold extracting sodium cyanide of a kind of sodium cyanide and lead sulfide, it utilize sodium cyanide desuifurized in the different physics-chem characteristic of each composition, the difference of solubleness in water particularly is with water as medium, by a series of separation and Extraction measures, make sodium cyanide break away from the water-soluble liquid cyanogen product that becomes fully, become the lead ore product after remaining waste residue filter is done.Though can make the waste residue compliance with environmental protection requirements, this method is not thoroughly eradicated the CN in the waste residue -, and only be that its content is controlled at the scope that is lower than 0.5ppm.At present also not about prepare the report of the method for zinc cyanide coproduction mixed sulfate with ammonia sodium method waste residue.
Summary of the invention
The invention provides a kind of method for preparing zinc cyanide coproduction mixed sulfate with ammonia sodium method waste residue; This method is not only with low cost, be easy to realize, and technology and production unit are simple, especially can thoroughly eradicate the CN in the waste residue -
To achieve the above object, technical scheme of the present invention is:
Ammonia sodium method waste residue prepares the method for zinc cyanide coproduction mixed sulfate, comprises being prepared as follows step:
Steps A, with the waste residue of ammonia sodium method gained, calculate with the sodium cyanide in the waste residue, put in the closed reaction kettle according to the mass ratio 1: 1.18~1.58 of pure substance, stir simultaneously with sodium sulfate, temperature in the reactor is controlled at 60~70 ℃, and stirring velocity is that per minute 30~60 changes; Slowly stir in the reactor and slowly generate new zinc cyanide and mixed sulfate down, this part reacts completely is that prussiate is reduced into zinc cyanide.
Step B, the mixture after reacting completely in the steps A is filtered with strainer;
Step C, will be among the step B filter the filter cake that obtains and burn;
Step D, deliver to and carry out low-temperature distillation in the underpressure distillation device filtering the filtrate obtain among the step B, distillation temperature is 60~70 ℃;
Step e, the liquid after the distillation among the step D is carried out crystallization through the low temperature crystallization device again, obtain zinc cyanide crystal and mixed sulfate successively.Low temperature crystallization at first obtains the zinc cyanide crystal, and remaining is mixed sulfate, can carry out deep processing when the quantity of vitriol accumulation increases, and is prepared into vitriol such as sodium sulfate, barium sulfate.
The present invention mainly is the waste residue that utilizes in the ammonia sodium method production process, when handling waste residue, prepare zinc cyanide coproduction mixed sulfate, because main technical schemes of the present invention is: ammonia sodium method waste residue and sodium sulfate placed earlier in the reactor of cryogenic seal react, obtaining filter cake impurity after the reaction after filtration sends to and incinerates, after filtrate is delivered to the underpressure distillation device and carried out low-temperature distillation, carry out crystallization through the low temperature crystallization device again; Make zinc cyanide crystal and mixed sulfate at last; Not only preparation technology is simple, and because the equipment used of the present invention has only reactor, suction filter, underpressure distillation device and crystallizer, so equipment also is simple and easy to; In addition, starting material utilize waste residue, and whole process mainly all is subzero treatment, and its energy consumption is lower and make it with low cost; Especially can thoroughly eradicate the CN in the waste residue -, eliminated of the pollution of the waste residue of prussiate production to environment, avoided taking limited soil and stacked, turn waste into wealth, make the waste residue content for rationally discharging up to standard, promptly reached environmental protection, create the prussiate and the Chemicals of certain economic value simultaneously again.
The chemically treated reaction principle of the present invention is:
2NaCN+ZnSO 4=====Zn(CN) 2+Na 2SO 4
Ba(CN) 2+ZnSO 4=====Zn(CN) 2+BaSO 4
Description of drawings
Fig. 1 is a process flow diagram of the present invention;
Wherein:
The 1--reactor, 2--strainer, 3--underpressure distillation device, 4--low temperature crystallization device, 5--zinc cyanide crystal, 6--mixed sulfate.
Concrete embodiment
Embodiment 1
Ammonia sodium method waste residue prepares the method for zinc cyanide coproduction mixed sulfate, comprises being prepared as follows step:
Steps A, with the waste residue of gained in the ammonia sodium method preparing product process, sodium cyanide in the waste residue is put in the closed reaction kettle 1 according to the mass ratio of pure substance with sodium sulfate in 200kg at 1: 1.18, stirs simultaneously, temperature in the reactor is controlled at 60 ℃, and stirring velocity is that per minute 60 changes;
Step B, the mixture after reacting completely in the steps A is filtered with strainer 2;
Step C, will be among the step B filter the filter cake that obtains and burn;
Step D, deliver to and carry out low-temperature distillation in the underpressure distillation device 3 filtering the filtrate obtain among the step B, distillation temperature is 60 ℃;
Step e, the liquid after the distillation among the step D is carried out crystallization through low temperature crystallization device 4 again, obtain 172.54kg zinc cyanide crystal 5 and 207.63kg sodium sulfate successively, sodium sulfate and zinc sulfate are handled the vitriol combination that other prussiate impurity (as barium cyanide) obtain and are obtained mixed sulfate 6.
Embodiment 2
Ammonia sodium method waste residue prepares the method for zinc cyanide coproduction mixed sulfate, comprises being prepared as follows step:
Steps A, with the waste residue of gained in the ammonia sodium method preparing product process, sodium cyanide in the waste residue 1: 1.38 is put into closed reaction kettle 1 with sodium sulfate according to the mass ratio of pure substance in 200kg, stirs simultaneously, temperature in the reactor is controlled at 65 ℃, and stirring velocity is that per minute 40 changes;
Step B, the mixture after reacting completely in the steps A is filtered with strainer 2;
Step C, will be among the step B filter the filter cake that obtains and burn;
Step D, deliver to and carry out low-temperature distillation in the underpressure distillation device 3 filtering the filtrate obtain among the step B, distillation temperature is 65 ℃;
Step e, the liquid after the distillation among the step D is carried out crystallization through low temperature crystallization device 4 again, obtain 201.78kg zinc cyanide crystal 5 and 242.83kg zinc sulfate successively, sodium sulfate and zinc sulfate are handled the vitriol combination that other prussiate impurity (as barium cyanide) obtain and are obtained mixed sulfate 6.
Embodiment 3
Ammonia sodium method waste residue prepares the method for zinc cyanide coproduction mixed sulfate, comprises being prepared as follows step:
Steps A, with the waste residue of gained in the ammonia sodium method preparing product process, sodium cyanide in the waste residue 1: 1.58 is put into closed reaction kettle 1 with sodium sulfate according to the mass ratio of pure substance in 200kg, stirs simultaneously, temperature in the reactor is controlled at 70 ℃, and stirring velocity is that per minute 30 changes;
Step B, the mixture after reacting completely in the steps A is filtered with strainer 2;
Step C, will be among the step B filter the filter cake that obtains and burn;
Step D, deliver to and carry out low-temperature distillation in the underpressure distillation device 3 filtering the filtrate obtain among the step B, distillation temperature is 70 ℃;
Step e, the liquid after the distillation among the step D is carried out crystallization through low temperature crystallization device 4 again, obtain 231.02kg zinc cyanide crystal 5 and 278.02kg zinc sulfate successively, sodium sulfate and zinc sulfate are handled the vitriol combination that other prussiate impurity (as barium cyanide) obtain and are obtained mixed sulfate 6.
The foregoing description is preferred embodiment of the present invention, is not to be used for limiting the scope of the present invention, so all equivalences of being done with described feature of claim of the present invention and principle change or modify, all should be included within the claim scope of the present invention.

Claims (2)

1. ammonia sodium method waste residue prepares the method for zinc cyanide coproduction mixed sulfate, it is characterized in that, comprises being prepared as follows step:
Steps A, with the waste residue of gained in the ammonia sodium method preparing product process, calculate with the sodium cyanide in the waste residue, put in the closed reaction kettle (1) according to the mass ratio 1: 1.18~1.58 of pure substance with sodium sulfate, stir simultaneously, the temperature in the reactor is controlled at 60~70 ℃;
Step B, the mixture after reacting completely in the steps A is filtered with strainer (2);
Step C, send to burning with filtering the filter cake obtain among the step B;
Step D, deliver in the underpressure distillation device (3) and carry out low-temperature distillation filtering the filtrate obtain among the step B, distillation temperature is 60~70 ℃;
Step e, the liquid after the distillation among the step D is passed through low temperature crystallization device (4) again and carries out crystallization, obtain zinc cyanide crystal (5) and vitriol (6) successively.
2. ammonia sodium method waste residue according to claim 1 prepares the method for zinc cyanide coproduction mixed sulfate, it is characterized in that, in the steps A, the stirring velocity in the described reactor is that per minute 30~60 changes.
CN 201010190357 2010-05-27 2010-05-27 Method for preparing zinc cyanide and jointly producing mixed sulfates from waste residues in Sodamide method Pending CN101955195A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104045096A (en) * 2014-05-04 2014-09-17 安徽盖娅环保科技有限公司 Method for preparing sodium cyanide and lead sulfide by separation of desulfurization slag produced from sodium cyanide production by light oil pyrolysis method
CN112125320A (en) * 2019-06-25 2020-12-25 湖南能也科技发展有限公司 Method for desalting water from barren liquor or barren liquor generated in gold extraction process by cyanidation

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5162200A (en) * 1974-11-28 1976-05-29 Koito Kogyo Kk KINZOKUSHIAN KABUTSUBUNRIHOHO
CN1254026A (en) * 1999-10-04 2000-05-24 郑晓廷 All-mud zinc cyanid powder substitution and carbon pulp adsorption seires-connection gold-extracting method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5162200A (en) * 1974-11-28 1976-05-29 Koito Kogyo Kk KINZOKUSHIAN KABUTSUBUNRIHOHO
CN1254026A (en) * 1999-10-04 2000-05-24 郑晓廷 All-mud zinc cyanid powder substitution and carbon pulp adsorption seires-connection gold-extracting method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
《江西冶金》 19921231 王庆民等 重选-重尾氰化锌置换提金工艺 第55~57页 1-2 第11卷, 第2期 2 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104045096A (en) * 2014-05-04 2014-09-17 安徽盖娅环保科技有限公司 Method for preparing sodium cyanide and lead sulfide by separation of desulfurization slag produced from sodium cyanide production by light oil pyrolysis method
CN104045096B (en) * 2014-05-04 2016-05-18 安徽盖娅环保科技有限公司 A kind of method of producing Cymag and vulcanized lead with the desuifurized separation that light oil cracking method production Cymag produces
CN112125320A (en) * 2019-06-25 2020-12-25 湖南能也科技发展有限公司 Method for desalting water from barren liquor or barren liquor generated in gold extraction process by cyanidation

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Application publication date: 20110126