CN102115138A - Method for preparing barium sulfate and co-producing potassium chloride with barium chloride waste slag - Google Patents
Method for preparing barium sulfate and co-producing potassium chloride with barium chloride waste slag Download PDFInfo
- Publication number
- CN102115138A CN102115138A CN 201010615456 CN201010615456A CN102115138A CN 102115138 A CN102115138 A CN 102115138A CN 201010615456 CN201010615456 CN 201010615456 CN 201010615456 A CN201010615456 A CN 201010615456A CN 102115138 A CN102115138 A CN 102115138A
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- China
- Prior art keywords
- barium
- chloride
- solution
- sulfate
- potassium chloride
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 title claims abstract description 35
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 title claims abstract description 34
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 title claims abstract description 32
- 229910001626 barium chloride Inorganic materials 0.000 title claims abstract description 32
- 239000002699 waste material Substances 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 17
- 239000001103 potassium chloride Substances 0.000 title claims abstract description 14
- 235000011164 potassium chloride Nutrition 0.000 title claims abstract 13
- 239000002893 slag Substances 0.000 title 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 23
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 22
- CJDPJFRMHVXWPT-UHFFFAOYSA-N barium sulfide Chemical compound [S-2].[Ba+2] CJDPJFRMHVXWPT-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 239000000047 product Substances 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 239000012065 filter cake Substances 0.000 claims abstract 4
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims abstract 4
- 229910052939 potassium sulfate Inorganic materials 0.000 claims abstract 4
- 235000011151 potassium sulphates Nutrition 0.000 claims abstract 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 6
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims 3
- 239000007789 gas Substances 0.000 claims 2
- 238000010521 absorption reaction Methods 0.000 claims 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims 1
- 238000001035 drying Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 238000005406 washing Methods 0.000 abstract 1
- 229940045511 barium chloride Drugs 0.000 description 16
- 239000011575 calcium Substances 0.000 description 4
- MVXMNHYVCLMLDD-UHFFFAOYSA-N 4-methoxynaphthalene-1-carbaldehyde Chemical compound C1=CC=C2C(OC)=CC=C(C=O)C2=C1 MVXMNHYVCLMLDD-UHFFFAOYSA-N 0.000 description 2
- 239000000920 calcium hydroxide Substances 0.000 description 2
- 235000011116 calcium hydroxide Nutrition 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- LBVNUQQORDPZCR-UHFFFAOYSA-N calcium;sulfane Chemical compound S.[Ca] LBVNUQQORDPZCR-UHFFFAOYSA-N 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000011085 pressure filtration Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention provides a method for preparing barium sulfate and coproducing potassium chloride by using barium chloride waste residues, wherein the barium chloride waste residues are waste residues obtained by preparing thiourea through the reaction of hydrochloric acid and barium sulfide, the barium chloride waste residues are fully dissolved in water and are mixed with the hydrochloric acid for reaction to obtain a solution containing barium chloride; mixing the solution containing barium chloride with potassium sulfate for reaction to obtain barium sulfate and potassium chloride; filtering to obtain a barium sulfate filter cake and a solution containing potassium chloride; washing, crushing and drying the barium sulfate filter cake to obtain a barium sulfate product; distilling the obtained solution containing potassium chloride to obtain supersaturated solution of potassium chloride, and crystallizing and separating out potassium chloride to obtain potassium chloride product. The method has simple operation and less equipment investment, converts the effective components in the barium sulfide waste residue into industrially usable substances, and is an economical and applicable method.
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 Repone K 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 Repone K 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 Repone K 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 vitriolate of tartar, and making the bariumchloride and the ratio of the molar content of the material of vitriolate of tartar is 1:0.8-1.2; Vitriolate of tartar and bariumchloride reaction generate barium sulfate and Repone K; After filtration, obtain barium sulfate filter cake and the solution that contains Repone K;
Step D: after barium sulfate filter cake washing, pulverizing and drying, obtain barium sulfate product;
Step e: with the solution distillation that contains Repone K of step C gained is the Repone K supersaturated solution, and the Repone K crystallization is separated out, and obtains the Repone K 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+K
2SO
4=====BaSO
4↓+2?KCl
Beneficial effect of the present invention is: the method for preparing barium sulfate and co-produced Repone K 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 Repone K 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 vitriolate of tartar, and making the bariumchloride and the ratio of the molar content of the material of vitriolate of tartar is 1:1.2; Vitriolate of tartar and bariumchloride reaction generate barium sulfate and Repone K; After filtration, obtain barium sulfate filter cake and the solution that contains Repone K;
Step D: after barium sulfate filter cake washing, pulverizing and drying, obtain barium sulfate product;
Step e: with the solution distillation that contains Repone K of step C gained is the Repone K supersaturated solution, and the Repone K crystallization is separated out, and obtains the Repone K product.
Embodiment 2:
Prepare the method for barium sulfate and co-produced Repone K 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 vitriolate of tartar, and making the bariumchloride and the ratio of the molar content of the material of vitriolate of tartar is 1:1; Vitriolate of tartar and bariumchloride reaction generate barium sulfate and Repone K; After filtration, obtain barium sulfate filter cake and the solution that contains Repone K;
Step D: after barium sulfate filter cake washing, pulverizing and drying, obtain barium sulfate product;
Step e: with the solution distillation that contains Repone K of step C gained is the Repone K supersaturated solution, and the Repone K crystallization is separated out, and obtains the Repone K product.
Embodiment 3:
Prepare the method for barium sulfate and co-produced Repone K 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 vitriolate of tartar, and making the bariumchloride and the ratio of the molar content of the material of vitriolate of tartar is 1:0.8; Vitriolate of tartar and bariumchloride reaction generate barium sulfate and Repone K; After filtration, obtain barium sulfate filter cake and the solution that contains Repone K;
Step D: after barium sulfate filter cake washing, pulverizing and drying, obtain barium sulfate product;
Step e: with the solution distillation that contains Repone K of step C gained is the Repone K supersaturated solution, and the Repone K crystallization is separated out, and obtains the Repone K 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)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010615456 CN102115138A (en) | 2010-12-31 | 2010-12-31 | Method for preparing barium sulfate and co-producing potassium chloride with barium chloride waste slag |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010615456 CN102115138A (en) | 2010-12-31 | 2010-12-31 | Method for preparing barium sulfate and co-producing potassium chloride with barium chloride waste slag |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102115138A true CN102115138A (en) | 2011-07-06 |
Family
ID=44214080
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010615456 Pending CN102115138A (en) | 2010-12-31 | 2010-12-31 | Method for preparing barium sulfate and co-producing potassium chloride with barium chloride waste slag |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102115138A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113371750A (en) * | 2021-06-08 | 2021-09-10 | 龙蟒佰利联集团股份有限公司 | Method for preparing barium sulfate by combining titanium white waste acid obtained by chlorination process and titanium white waste acid obtained by sulfuric acid process |
-
2010
- 2010-12-31 CN CN 201010615456 patent/CN102115138A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 《河北化工》 19990131 郭斌等 含钡废渣酸浸法制取硫酸钡 第1、2、3.1节 1 , 第1期 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113371750A (en) * | 2021-06-08 | 2021-09-10 | 龙蟒佰利联集团股份有限公司 | Method for preparing barium sulfate by combining titanium white waste acid obtained by chlorination process and titanium white waste acid obtained by sulfuric acid process |
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| PB01 | Publication | ||
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Application publication date: 20110706 |