CN102115135A - Method for preparing barium sulfate coproduced with ferrous chloride by using barium chloride waste residues - Google Patents
Method for preparing barium sulfate coproduced with ferrous chloride by using barium chloride waste residues Download PDFInfo
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- CN102115135A CN102115135A CN 201010615443 CN201010615443A CN102115135A CN 102115135 A CN102115135 A CN 102115135A CN 201010615443 CN201010615443 CN 201010615443 CN 201010615443 A CN201010615443 A CN 201010615443A CN 102115135 A CN102115135 A CN 102115135A
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- barium
- bariumchloride
- solution
- ferrous
- barium sulfate
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Abstract
The invention provides a method for preparing barium sulfate coproduced with ferrous chloride by using barium chloride waste residues. The method comprises the following steps of: fully dissolving barium chloride waste residues produced during the preparation of thiourea by making hydrochloric acid react with barium sulfide, and making the solution react with hydrochloric acid by mixing to obtain a barium chloride-containing solution; making the barium chloride-containing solution react with ferrous sulfate by mixing to obtain barium sulfate and ferrous chloride; filtering to obtain a barium sulfate filter cake and a solution containing ferrous chloride; washing the barium sulfate filter cake, grinding and drying to obtain a barium sulfate product; and distilling the solution containing ferrous chloride to obtain a supersaturated ferrous chloride solution, and separating ferrous chloride crystals out to obtain a ferrous chloride product. The method is easy to operate, has small equipment investment, is used for transforming active ingredients in barium chloride waste residues into an industrially usable substance, and is economical and applicable.
Description
Technical field
The present invention relates to the disposal of three wastes of inorganic chemical industry thiocarbamide manufacturing and utilize technical field, especially prepare the method for barium sulfate and co-produced iron protochloride with the bariumchloride waste residue, described is the waste residue of hydrochloric acid and barium sulphide prepared in reaction thiocarbamide gained with the bariumchloride waste residue.
Background technology
The production method of thiocarbamide is a lot, wherein traditional method is to utilize barium sulphide and hydrochloric acid reaction to generate hydrogen sulfide and bariumchloride precipitation, hydrogen sulfide absorbs through the milk of lime negative pressure and makes the hydrogen sulfide calcium solution, then react with calcium cyanamide again, the mol ratio of calcium sulfhydrate and calcium cyanamide is 1: 5, under constantly stirring, temperature of reaction is (80 ± 5) ℃, reaction times is 3h, through negative pressure filtration, can generate thiocarbamide liquid, again through evaporation, filtration, cooling, crystallization, promptly get the crystal thiocarbamide, centrifugal drying gets product.Reaction equation is as follows:
BaS+2HCl→BaC12+H2S↑
CaO+H2O→Ca(OH)2
2H
2S+Ca(OH)
2→Ca(SH)
2+2H
2O
2CaCN
2+Ca(SH
2)
2+6H
2O→2(NH
2)
2CS+3Ca(OH)
2
Aforesaid method is produced thiocarbamide, and its main industrial residue is exactly the bariumchloride waste residue, according to one's analysis, also contains a large amount of barium sulphides in the bariumchloride waste residue.
Summary of the invention
The waste residue of hydrochloric acid and barium sulphide prepared in reaction thiocarbamide gained is bariumchloride waste residue of the present invention, and its main component is a bariumchloride, also contains a large amount of barium sulphides, the invention provides the method for preparing common barium sulfate and iron protochloride with above-mentioned bariumchloride waste residue.This method is simple to operate, and facility investment is few, and the effective constituent in the bariumchloride waste residue is converted into industrial utilizable material, is an economic and practical method.
Technical scheme of the present invention is as follows: prepare the method for barium sulfate and co-produced iron protochloride with the bariumchloride waste residue, described is the waste residue of hydrochloric acid and barium sulphide prepared in reaction thiocarbamide gained with the bariumchloride waste residue, comprises following concrete steps:
Steps A: the bariumchloride waste residue fully is dissolved in water, is mainly contained the solution of bariumchloride and barium sulphide, convert the wherein molar content of barium sulphide;
Step B: with the steps A gained mainly contain bariumchloride and barium sulfide solution mixes with excessive hydrochloric acid, the molar content that makes barium sulphide is 1:1.6-2.4 with the ratio of the molar content of hydrogenchloride, hydrochloric acid and barium sulphide reaction generate bariumchloride and hydrogen sulfide, after hydrogen sulfide is overflowed from solution, obtain containing the solution of bariumchloride, the effusion hydrogen sulfide feeds in the sodium hydroxide solution and absorbs, in order to avoid contaminate environment;
Step C: the solution that contains bariumchloride and small amount of hydrochloric acid of step B gained is mixed with ferrous sulfate, and making the bariumchloride and the ratio of the molar content of the material of ferrous sulfate is 1:0.8-1.2; Ferrous sulfate and bariumchloride reaction generate barium sulfate and iron protochloride; After filtration, obtain the barium sulfate filter cake and contain chlorination ferrous solution;
Step D: after barium sulfate filter cake washing, pulverizing and drying, obtain barium sulfate product;
Step e: the chlorination ferrous solution distillation of containing of step C gained is the iron protochloride supersaturated solution, the iron protochloride crystallization is separated out, obtain the iron protochloride product.
Of the present inventionly prepare the method for barium sulfate and co-produced ammonia chloride with the bariumchloride waste residue, related chemical principle is:
BaS+2HCl=====BaCl
2+H
2S
BaCl
2+FeSO
4=====BaSO
4↓+2FeCl2
Beneficial effect of the present invention is: the method for preparing barium sulfate and co-produced iron protochloride with the bariumchloride waste residue of the present invention, this method is simple to operate, facility investment is few, and the effective constituent in the bariumchloride waste residue is converted into industrial utilizable material, is an economic and practical method.
Embodiment
Embodiment 1:
Prepare the method for barium sulfate and co-produced iron protochloride with the bariumchloride waste residue, described is the waste residue of hydrochloric acid and barium sulphide prepared in reaction thiocarbamide gained with the bariumchloride waste residue, comprises following concrete steps:
Steps A: 500kg bariumchloride waste residue fully is dissolved in water, is mainly contained the solution of bariumchloride and barium sulphide, convert the wherein molar content of barium sulphide;
Step B: the steps A gained mainly contained bariumchloride and barium sulfide solution and mixed in hydrochloric acid, the molar content that makes barium sulphide is 1:1.6 with the ratio of the molar content of hydrogenchloride, hydrochloric acid and barium sulphide reaction generate bariumchloride and hydrogen sulfide, after hydrogen sulfide is overflowed from solution, obtain containing the solution of bariumchloride, the effusion hydrogen sulfide feeds in the sodium hydroxide solution and absorbs, in order to avoid contaminate environment;
Step C: the solution that contains bariumchloride and small amount of hydrochloric acid of step B gained is mixed with ferrous sulfate, and making the bariumchloride and the ratio of the molar content of the material of ferrous sulfate is 1:1.2; Ferrous sulfate and bariumchloride reaction generate barium sulfate and iron protochloride; After filtration, obtain the barium sulfate filter cake and contain chlorination ferrous solution;
Step D: after barium sulfate filter cake washing, pulverizing and drying, obtain barium sulfate product;
Step e: the chlorination ferrous solution distillation of containing of step C gained is the iron protochloride supersaturated solution, the iron protochloride crystallization is separated out, obtain the iron protochloride product.
Embodiment 2:
Prepare the method for barium sulfate and co-produced iron protochloride with the bariumchloride waste residue, described is the waste residue of hydrochloric acid and barium sulphide prepared in reaction thiocarbamide gained with the bariumchloride waste residue, comprises following concrete steps:
Steps A: 500kg bariumchloride waste residue fully is dissolved in water, is mainly contained the solution of bariumchloride and barium sulphide, convert the wherein molar content of barium sulphide;
Step B: the steps A gained mainly contained bariumchloride and barium sulfide solution and mixed in hydrochloric acid, the molar content that makes barium sulphide is 1:2 with the ratio of the molar content of hydrogenchloride, hydrochloric acid and barium sulphide reaction generate bariumchloride and hydrogen sulfide, after hydrogen sulfide is overflowed from solution, obtain containing the solution of bariumchloride, the effusion hydrogen sulfide feeds in the sodium hydroxide solution and absorbs, in order to avoid contaminate environment;
Step C: the solution that contains bariumchloride and small amount of hydrochloric acid of step B gained is mixed with ferrous sulfate, and making the bariumchloride and the ratio of the molar content of the material of ferrous sulfate is 1:1; Ferrous sulfate and bariumchloride reaction generate barium sulfate and iron protochloride; After filtration, obtain the barium sulfate filter cake and contain chlorination ferrous solution;
Step D: after barium sulfate filter cake washing, pulverizing and drying, obtain barium sulfate product;
Step e: the chlorination ferrous solution distillation of containing of step C gained is the iron protochloride supersaturated solution, the iron protochloride crystallization is separated out, obtain the iron protochloride product.
Embodiment 3:
Prepare the method for barium sulfate and co-produced iron protochloride with 500kg bariumchloride waste residue, described is the waste residue of hydrochloric acid and barium sulphide prepared in reaction thiocarbamide gained with the bariumchloride waste residue, comprises following concrete steps:
Steps A: the bariumchloride waste residue fully is dissolved in water, is mainly contained the solution of bariumchloride and barium sulphide, convert the wherein molar content of barium sulphide;
Step B: the steps A gained mainly contained bariumchloride and barium sulfide solution and mixed in hydrochloric acid, the molar content that makes barium sulphide is 1:2.4 with the ratio of the molar content of hydrogenchloride, hydrochloric acid and barium sulphide reaction generate bariumchloride and hydrogen sulfide, after hydrogen sulfide is overflowed from solution, obtain containing the solution of bariumchloride, the effusion hydrogen sulfide feeds in the sodium hydroxide solution and absorbs, in order to avoid contaminate environment;
Step C: the solution that contains bariumchloride and small amount of hydrochloric acid of step B gained is mixed with ferrous sulfate, and making the bariumchloride and the ratio of the molar content of the material of ferrous sulfate is 1:0.8; Ferrous sulfate and bariumchloride reaction generate barium sulfate and iron protochloride; After filtration, obtain the barium sulfate filter cake and contain chlorination ferrous solution;
Step D: after barium sulfate filter cake washing, pulverizing and drying, obtain barium sulfate product;
Step e: the chlorination ferrous solution distillation of containing of step C gained is the iron protochloride supersaturated solution, the iron protochloride crystallization is separated out, obtain the iron protochloride product.
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. prepare the method for barium sulfate and co-produced iron protochloride with the bariumchloride waste residue, it is characterized in that, described is the waste residue of hydrochloric acid and barium sulphide prepared in reaction thiocarbamide gained with the bariumchloride waste residue, comprises following concrete steps:
Steps A: the bariumchloride waste residue fully is dissolved in water, is mainly contained the solution of bariumchloride and barium sulphide, convert the wherein molar content of barium sulphide;
Step B: the steps A gained mainly contained bariumchloride and barium sulfide solution and mixed in hydrochloric acid, the molar content that makes barium sulphide is 1:1.6-2.4 with the ratio of the molar content of hydrogenchloride, hydrochloric acid and barium sulphide reaction generate bariumchloride and hydrogen sulfide, after hydrogen sulfide is overflowed from solution, obtain containing the solution of bariumchloride, the effusion hydrogen sulfide feeds in the sodium hydroxide solution and absorbs, in order to avoid contaminate environment;
Step C: the solution that contains bariumchloride and small amount of hydrochloric acid of step B gained is mixed with ferrous sulfate, and making the bariumchloride and the ratio of the molar content of the material of ferrous sulfate is 1:0.8-1.2; Ferrous sulfate and bariumchloride reaction generate barium sulfate and iron protochloride; After filtration, obtain the barium sulfate filter cake and contain chlorination ferrous solution;
Step D: after barium sulfate filter cake washing, pulverizing and drying, obtain barium sulfate product;
Step e: the chlorination ferrous solution distillation of containing of step C gained is the iron protochloride supersaturated solution, the iron protochloride crystallization is separated out, obtain the iron protochloride product.
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|---|---|---|---|
| CN 201010615443 CN102115135A (en) | 2010-12-31 | 2010-12-31 | Method for preparing barium sulfate coproduced with ferrous chloride by using barium chloride waste residues |
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| CN 201010615443 CN102115135A (en) | 2010-12-31 | 2010-12-31 | Method for preparing barium sulfate coproduced with ferrous chloride by using barium chloride waste residues |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109970089A (en) * | 2019-05-20 | 2019-07-05 | 长沙中硅水泥技术开发有限公司 | A kind of method and system preparing barium sulfate using barium slag |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85107743A (en) * | 1985-10-18 | 1986-10-15 | 太原工业大学 | Co-producing sulfuric acid barium and magnesian hydrochloric acid cyclic method |
| US5312604A (en) * | 1990-05-31 | 1994-05-17 | Kali-Chemie Ag | Work-up of waste materials from barium or strontium sulfide leaching |
| CN101643233A (en) * | 2009-06-08 | 2010-02-10 | 王嘉兴 | Method for preparing co-production sodium chloride of precipitated barium sulfate |
| CN101850999A (en) * | 2009-04-13 | 2010-10-06 | 王嘉兴 | Method for preparing micro fine precipitated barium sulfate and co-producing hydrochloric acid by using barium slag |
-
2010
- 2010-12-31 CN CN 201010615443 patent/CN102115135A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85107743A (en) * | 1985-10-18 | 1986-10-15 | 太原工业大学 | Co-producing sulfuric acid barium and magnesian hydrochloric acid cyclic method |
| US5312604A (en) * | 1990-05-31 | 1994-05-17 | Kali-Chemie Ag | Work-up of waste materials from barium or strontium sulfide leaching |
| CN101850999A (en) * | 2009-04-13 | 2010-10-06 | 王嘉兴 | Method for preparing micro fine precipitated barium sulfate and co-producing hydrochloric acid by using barium slag |
| CN101643233A (en) * | 2009-06-08 | 2010-02-10 | 王嘉兴 | Method for preparing co-production sodium chloride of precipitated barium sulfate |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109970089A (en) * | 2019-05-20 | 2019-07-05 | 长沙中硅水泥技术开发有限公司 | A kind of method and system preparing barium sulfate using barium slag |
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Application publication date: 20110706 |