CN102115139A - Method for producing barium sulfate and ammonia chloride by using barium chloride waste residue - Google Patents
Method for producing barium sulfate and ammonia chloride by using barium chloride waste residue Download PDFInfo
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- CN102115139A CN102115139A CN 201010615460 CN201010615460A CN102115139A CN 102115139 A CN102115139 A CN 102115139A CN 201010615460 CN201010615460 CN 201010615460 CN 201010615460 A CN201010615460 A CN 201010615460A CN 102115139 A CN102115139 A CN 102115139A
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- barium
- bariumchloride
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- waste residue
- sulfate
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Abstract
The invention provides a method for producing barium sulfate and ammonia chloride by using barium chloride waste residue, which comprises: fully dissolving barium chloride waste residue from the preparation of thiourea by the reaction of hydrochloric acid and barium sulfide in water, and mixing the solution with hydrochloric acid for reaction to obtain solution containing barium chloride; mixing the solution containing barium chloride with ammonium sulfate for reaction to obtain barium sulfate and ammonium chloride; filtering to obtain a barium sulfate filter cake and solution containing ammonium chloride; washing, crushing and drying the barium sulfate filter cake to obtain a barium sulfate product; and distilling the obtained solution containing ammonium chloride to obtain oversaturated solution, and crystallizing and precipitating ammonium chloride to obtain an ammonium chloride product. In the method, operation is simple, equipment investment is low, and active ingredients in barium chloride waste residue are converted into materials that can be used in industry. Thus, the method is economic 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 ammonia chloride 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 ammonia chloride 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 ammonia chloride 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 sulfate of ammoniac, and making the bariumchloride and the ratio of the molar content of the material of sulfate of ammoniac is 1:0.8-1.2; Sulfate of ammoniac and bariumchloride reaction generate barium sulfate and ammonia chloride; After filtration, obtain barium sulfate filter cake and the solution that contains ammonia chloride;
Step D: after barium sulfate filter cake washing, pulverizing and drying, obtain barium sulfate product;
Step e: with the solution distillation that contains ammonia chloride of step C gained is the ammonia chloride supersaturated solution, and the ammonia chloride crystallization is separated out, and obtains the ammonia chloride 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+(NH4)
2SO
4=====BaSO
4↓+2NH4Cl
Beneficial effect of the present invention is: the method for preparing barium sulfate and co-produced ammonia chloride 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 ammonia chloride 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 of step B gained is mixed with sulfate of ammoniac, and making the bariumchloride and the ratio of the molar content of the material of sulfate of ammoniac is 1:1.2; Sulfate of ammoniac and bariumchloride reaction generate barium sulfate and ammonia chloride; After filtration, obtain barium sulfate filter cake and the solution that contains ammonia chloride;
Step D: after barium sulfate filter cake washing, pulverizing and drying, obtain barium sulfate product;
Step e: with the solution distillation that contains ammonia chloride of step C gained is the ammonia chloride supersaturated solution, and the ammonia chloride crystallization is separated out, and obtains the ammonia chloride product.
Embodiment 2:
Prepare the method for barium sulfate and co-produced ammonia chloride 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 of step B gained is mixed with sulfate of ammoniac, and making the bariumchloride and the ratio of the molar content of the material of sulfate of ammoniac is 1:1; Sulfate of ammoniac and bariumchloride reaction generate barium sulfate and ammonia chloride; After filtration, obtain barium sulfate filter cake and the solution that contains ammonia chloride;
Step D: after barium sulfate filter cake washing, pulverizing and drying, obtain barium sulfate product;
Step e: with the solution distillation that contains ammonia chloride of step C gained is the ammonia chloride supersaturated solution, and the ammonia chloride crystallization is separated out, and obtains the ammonia chloride product.
Embodiment 3:
Prepare the method for barium sulfate and co-produced ammonia chloride 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 of step B gained is mixed with sulfate of ammoniac, and making the bariumchloride and the ratio of the molar content of the material of sulfate of ammoniac is 1:0.8; Sulfate of ammoniac and bariumchloride reaction generate barium sulfate and ammonia chloride; After filtration, obtain barium sulfate filter cake and the solution that contains ammonia chloride;
Step D: after barium sulfate filter cake washing, pulverizing and drying, obtain barium sulfate product;
Step e: with the solution distillation that contains ammonia chloride of step C gained is the ammonia chloride supersaturated solution, and the ammonia chloride crystallization is separated out, and obtains the ammonia chloride 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 ammonia chloride 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 of step B gained is mixed with sulfate of ammoniac, and making the bariumchloride and the ratio of the molar content of the material of sulfate of ammoniac is 1:0.8-1.2; Sulfate of ammoniac and bariumchloride reaction generate barium sulfate and ammonia chloride; After filtration, obtain barium sulfate filter cake and the solution that contains ammonia chloride;
Step D: after barium sulfate filter cake washing, pulverizing and drying, obtain barium sulfate product;
Step e: with the solution distillation that contains ammonia chloride of step C gained is the ammonia chloride supersaturated solution, and the ammonia chloride crystallization is separated out, and obtains the ammonia chloride product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106154607A CN102115139B (en) | 2010-12-31 | 2010-12-31 | Method for producing barium sulfate and ammonia chloride by using barium chloride waste residue |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106154607A CN102115139B (en) | 2010-12-31 | 2010-12-31 | Method for producing barium sulfate and ammonia chloride by using barium chloride waste residue |
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| Publication Number | Publication Date |
|---|---|
| CN102115139A true CN102115139A (en) | 2011-07-06 |
| CN102115139B CN102115139B (en) | 2012-11-07 |
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| Application Number | Title | Priority Date | Filing Date |
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Citations (2)
| 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 |
| CN1342612A (en) * | 2001-10-15 | 2002-04-03 | 广西大学 | Process for preparing both barium sulfate and calcium chloride from waste ardealite dregs |
-
2010
- 2010-12-31 CN CN2010106154607A patent/CN102115139B/en active Active
Patent Citations (2)
| 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 |
| CN1342612A (en) * | 2001-10-15 | 2002-04-03 | 广西大学 | Process for preparing both barium sulfate and calcium chloride from waste ardealite dregs |
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| Publication number | Publication date |
|---|---|
| CN102115139B (en) | 2012-11-07 |
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Owner name: RUGAO LEHENG CHEMICAL CO., LTD. Free format text: FORMER OWNER: XIE SHANQING Effective date: 20130912 |
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Effective date of registration: 20130912 Address after: 226500 No. 8, Pujiang Road, Changjiang town (Rugao port area), Jiangsu, Rugao Patentee after: Rugao City Leheng Chemical Company Ltd. Address before: 10, Guangdong, Dongguan province Dongcheng District vortex mountain commercial street, No. 523008, ladder 703 Patentee before: Xie Shanqing |