CN111204803A - Zirconium sulfate solution and production process thereof - Google Patents
Zirconium sulfate solution and production process thereof Download PDFInfo
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- CN111204803A CN111204803A CN202010149298.8A CN202010149298A CN111204803A CN 111204803 A CN111204803 A CN 111204803A CN 202010149298 A CN202010149298 A CN 202010149298A CN 111204803 A CN111204803 A CN 111204803A
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- CN
- China
- Prior art keywords
- zirconium
- solution
- zirconium sulfate
- sulfate solution
- sulfuric acid
- 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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- ZXAUZSQITFJWPS-UHFFFAOYSA-J zirconium(4+);disulfate Chemical compound [Zr+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZXAUZSQITFJWPS-UHFFFAOYSA-J 0.000 title claims abstract description 70
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 30
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 46
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 claims abstract description 30
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical group [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000003381 stabilizer Substances 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 239000007787 solid Substances 0.000 claims description 8
- 239000012535 impurity Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 abstract description 14
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 abstract description 9
- 238000001953 recrystallisation Methods 0.000 abstract description 9
- 229910052726 zirconium Inorganic materials 0.000 abstract description 9
- 238000002425 crystallisation Methods 0.000 abstract description 8
- 239000002699 waste material Substances 0.000 abstract description 8
- 230000008025 crystallization Effects 0.000 abstract description 7
- ATYZRBBOXUWECY-UHFFFAOYSA-N zirconium;hydrate Chemical compound O.[Zr] ATYZRBBOXUWECY-UHFFFAOYSA-N 0.000 abstract 1
- 238000011084 recovery Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N hydrochloric acid Substances Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 239000010985 leather Substances 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910017344 Fe2 O3 Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000005903 acid hydrolysis reaction Methods 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- PANBYUAFMMOFOV-UHFFFAOYSA-N sodium;sulfuric acid Chemical compound [Na].OS(O)(=O)=O PANBYUAFMMOFOV-UHFFFAOYSA-N 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910052845 zircon Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
- C01G25/06—Sulfates
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a zirconium sulfate solution and a production process thereof, wherein the zirconium sulfate solution contains 110-115g/L zirconium sulfate, a stabilizing agent is added in the zirconium sulfate solution, the stabilizing agent is anhydrous sodium sulfate, and the mass ratio of the anhydrous sodium sulfate to the zirconium sulfate solution is 2: 100, respectively; the production process of the zirconium sulfate solution comprises the following steps: (1) dissolving zirconium oxychloride and water in a mass ratio of 1: 2.5-3; (2) filtering the zirconium oxychloride solution; (3) the volume ratio of the zirconium oxychloride solution is 5: 1 adding concentrated sulfuric acid with the concentration of 98%; (4) adding a stabilizer anhydrous sodium sulfate into the zirconium sulfate solution, wherein the mass ratio of the anhydrous sodium sulfate to the zirconium sulfate solution is 2: 100. the product and the production process thereof can improve the utilization rate of zirconium, reduce crystallization and recrystallization procedures, reduce the use of sulfuric acid, have no waste liquid, reduce the treatment cost, have good solution stability and are convenient for downstream customers to use.
Description
Technical Field
The invention relates to zirconium sulfate, in particular to a zirconium sulfate solution and a production process thereof.
Background
Zirconium sulfate is mainly used as a protein precipitator and a tanning agent for leather such as white leather, wrinkled leather and the like, can also be used as a catalyst and an anti-abrasion agent, and is widely applied in modern industrial production.
The method for producing zirconium sulfate from zircon comprises the following steps: (1) zircon-sintering or alkali fusion-washing-sulfuric acid leaching-ammonia water precipitation-washing to remove sodium-sulfuric acid dissolution-evaporative crystallization-recrystallization-zirconium sulfate product. (2) Zircon-alkali fusion-washing-hydrochloric acid leaching-hydrolysis-sulfuric acid dissolution-crystallization-zirconium sulfate product.
The first method has long process flow, low metal recovery rate, zirconium recovery rate generally below 70 percent, unstable product quality and high production cost.
The second method uses hydrochloric acid, so that the equipment is seriously corroded and the operating environment is poor. Because the low acid eel has high acid hydrolysis, the metal recovery rate is low, and the titanium content of the product is higher.
In addition, zirconium sulfate can also be produced from zirconium oxychloride, namely: zirconium oxychloride-dissolution-crystallization with sulfuric acid- (recrystallization) -zirconium sulfate product. The recrystallization needs to concentrate the solution and add sulfuric acid again, the production process is complex, and in the process of recrystallization, because the impurity content in the solution after primary crystallization is higher, the impurity content of the recrystallized product is higher, and the quality is poor.
The zirconium sulfate produced by zirconium oxychloride has the advantages that in the production process, the recovery rate of zirconium is low, more sulfuric acid is consumed in the production process, the waste liquid generated in the production process needs to be treated and then discharged, and the cost is high.
In summary, the problems of the existing solid zirconium sulfate products are as follows:
in the production process, the process is more complicated and complicated, and specifically:
1. hydrogen chloride gas is discharged in the reaction process, and air pollution is serious.
2. About 1 ton of dilute sulfuric acid is produced per ton of zirconium sulfate, and the dilute sulfuric acid is difficult to process.
3. The zirconium oxychloride raw material consumed by producing each ton of zirconium sulfate is large, and the recovery rate is low.
4. The waste liquid after production needs special treatment, and has high cost and large expense.
In addition, after production, downstream users can use the liquid after dissolving the liquid before using the liquid, which is inconvenient for production and use and consumes water resources.
Disclosure of Invention
The invention aims to solve the technical problem of providing a zirconium sulfate solution and a production process thereof, wherein the zirconium sulfate solution can be produced by improving the utilization rate of zirconium, reducing crystallization and recrystallization procedures, reducing the use of sulfuric acid, generating no waste liquid, reducing the treatment cost, facilitating the use of downstream customers and reducing the consumption of water resources.
In order to solve the technical problems, the invention adopts the following technical means:
a zirconium sulfate solution is provided, wherein the content of zirconium sulfate in the zirconium sulfate solution is 110-115g/L, a stabilizing agent is added in the zirconium sulfate solution, the stabilizing agent is anhydrous sodium sulfate, and the mass ratio of the anhydrous sodium sulfate to the zirconium sulfate solution is 2: 100.
in the prior art, the reaction temperature is about 115 ℃, the use amount of sulfuric acid is large, while the reaction temperature of the zirconium sulfate solution is lower than 100 ℃ in the production process, and the added sulfuric acid amount is small, so that compared with the prior art, the zirconium sulfate solution produced by the method can improve the utilization rate of zirconium, reduce crystallization and recrystallization processes, reduce the use of sulfuric acid, avoid the generation of waste liquid, reduce the treatment cost and reduce the production cost by about 8%; and the system is convenient for downstream customers to use, and reduces the water resource consumption.
The production process of the zirconium sulfate solution comprises the following steps:
(1) dissolving zirconium oxychloride in water to obtain a zirconium oxychloride solution, wherein the mass ratio of the zirconium oxychloride to the water is 1: 2.5-3;
(2) filtering the zirconium oxychloride solution to remove solid insoluble impurities;
(3) adding concentrated sulfuric acid into a zirconium oxychloride solution to obtain a zirconium sulfate solution, wherein the concentration of the concentrated sulfuric acid is 98%, and the volume ratio of the zirconium oxychloride solution to the concentrated sulfuric acid is 5: 1;
(4) adding a stabilizer anhydrous sodium sulfate into the zirconium sulfate solution, wherein the mass ratio of the anhydrous sodium sulfate to the zirconium sulfate solution is 2: 100.
the production process can improve the utilization rate of zirconium, reduce crystallization and recrystallization procedures, reduce the use of sulfuric acid, avoid the generation of waste liquid, reduce the treatment cost, facilitate the use of downstream customers and reduce the consumption of water resources. The stabilizer anhydrous sodium sulfate is added into the zirconium sulfate solution, so that the stability of the solution can be effectively improved, and the use of downstream customers is facilitated.
In the production process of the zirconium sulfate solution, when concentrated sulfuric acid is added into the zirconium oxychloride solution in the step (3), the reaction temperature is not more than 98 ℃.
In the production process of the zirconium sulfate solution, when concentrated sulfuric acid is added into the zirconium oxychloride solution in the step (3), the reaction temperature is 90 ℃.
The reaction temperature was controlled not to exceed 98 ℃ by controlling the rate of addition of sulfuric acid.
Detailed Description
The present invention will be further described with reference to the following examples.
A zirconium sulfate solution is provided, wherein the content of zirconium sulfate in the zirconium sulfate solution is 110-115g/L, a stabilizing agent is added in the zirconium sulfate solution, the stabilizing agent is anhydrous sodium sulfate, and the mass ratio of the anhydrous sodium sulfate to the zirconium sulfate solution is 2: 100.
the zirconium sulfate solution is produced, the utilization rate of zirconium can be improved, the crystallization and recrystallization processes are reduced, the use of sulfuric acid is reduced, no waste liquid is generated, the treatment cost is reduced, the zirconium sulfate solution is convenient for downstream customers to use, and the consumption of water resources is reduced.
The production process of the zirconium sulfate solution comprises the following steps:
(1) dissolving zirconium oxychloride in water to obtain a zirconium oxychloride solution, wherein the mass ratio of the zirconium oxychloride to the water is 1: 2.5-3;
(2) filtering the zirconium oxychloride solution to remove solid insoluble impurities;
(3) adding concentrated sulfuric acid into a zirconium oxychloride solution to obtain a zirconium sulfate solution, wherein the concentration of the concentrated sulfuric acid is 98%, and the volume ratio of the zirconium oxychloride solution to the concentrated sulfuric acid is 5: 1;
(4) adding a stabilizer anhydrous sodium sulfate into the zirconium sulfate solution, wherein the mass ratio of the anhydrous sodium sulfate to the zirconium sulfate solution is 2: 100.
the production process can improve the utilization rate of zirconium, reduce crystallization and recrystallization procedures, reduce the use of sulfuric acid, avoid the generation of waste liquid, reduce the treatment cost, facilitate the use of downstream customers and reduce the consumption of water resources. The stabilizer anhydrous sodium sulfate is added into the zirconium sulfate solution, so that the stability of the solution can be effectively improved, and the use of downstream customers is facilitated.
In the production process of the zirconium sulfate solution, when concentrated sulfuric acid is added into the zirconium oxychloride solution in the step (3), the reaction temperature is not more than 98 ℃.
In the production process of the zirconium sulfate solution, when concentrated sulfuric acid is added into the zirconium oxychloride solution in the step (3), the reaction temperature is 90 ℃.
The reaction temperature was controlled not to exceed 98 ℃ by controlling the rate of addition of sulfuric acid.
The comparison table of the performance indexes of the zirconium sulfate solution processed according to the process is as follows:
| ZrO2(g/l) | Fe2 O3（ppm） | specific gravity of the solution | |
| After the solid zirconium sulfate is dissolved | 102 | 8.3 | 1.2 |
| Zirconium sulfate solution of the invention | 105 | 5.6 | 1.2 |
As can be seen from the above table, ZrO of the present product was obtained under the condition that the specific gravities of the solutions were the same2The content is higher than that of dissolved solid zirconium sulfate, Fe2O3The content of (b) is lower than the content of dissolved solid zirconium sulfate.
Namely: the zirconium sulfate solution of the present invention is superior to solutions in which solid zirconium sulfate is dissolved.
The liquid zirconium sulfate produced by the invention is used by more than 3000 tons by customers, the use effect of the liquid zirconium sulfate is approved and confirmed by users, and the liquid zirconium sulfate is comprehensively popularized and used.
The above description is only for the purpose of illustrating preferred embodiments of the present invention and is not intended to limit the scope of the present invention, which is defined by the appended claims.
Claims (4)
1. A zirconium sulfate solution characterized by: in the zirconium sulfate solution, the content of zirconium sulfate is 110-115g/L, a stabilizing agent is added in the zirconium sulfate solution, the stabilizing agent is anhydrous sodium sulfate, and the mass ratio of the anhydrous sodium sulfate to the zirconium sulfate solution is 2: 100.
2. the process for the production of a zirconium sulfate solution according to claim 1, characterized by comprising the steps of:
(1) dissolving zirconium oxychloride in water to obtain a zirconium oxychloride solution, wherein the mass ratio of the zirconium oxychloride to the water is 1: 2.5-3;
(2) filtering the zirconium oxychloride solution to remove solid insoluble impurities;
(3) adding concentrated sulfuric acid into a zirconium oxychloride solution to obtain a zirconium sulfate solution, wherein the concentration of the concentrated sulfuric acid is 98%, and the volume ratio of the zirconium oxychloride solution to the concentrated sulfuric acid is 5: 1;
(4) adding a stabilizer anhydrous sodium sulfate into the zirconium sulfate solution, wherein the mass ratio of the anhydrous sodium sulfate to the zirconium sulfate solution is 2: 100.
3. the process for the production of a zirconium sulfate solution according to claim 2, characterized in that: when concentrated sulfuric acid is added into the zirconium oxychloride solution in the step (3), the reaction temperature is not more than 98 ℃.
4. The process for the production of a zirconium sulfate solution according to claim 3, characterized in that: when concentrated sulfuric acid is added into the zirconium oxychloride solution in the step (3), the reaction temperature is 90 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010149298.8A CN111204803A (en) | 2020-03-06 | 2020-03-06 | Zirconium sulfate solution and production process thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010149298.8A CN111204803A (en) | 2020-03-06 | 2020-03-06 | Zirconium sulfate solution and production process thereof |
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| CN111204803A true CN111204803A (en) | 2020-05-29 |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1316107A (en) * | 1918-07-15 | 1919-09-16 | Pennsylvania Salt Mfg Co | Basic sulfate of zirconium and method of making the same. |
| GB606681A (en) * | 1944-05-11 | 1948-08-18 | Produits Chim Terres Rares Soc | An improved method for obtaining industrially pure double sodium zirconium sulphates |
| US5470550A (en) * | 1993-12-30 | 1995-11-28 | Westinghouse Electric Corporation | Zirconium sulfate precipitation |
| US6358484B1 (en) * | 2000-03-31 | 2002-03-19 | Ati Properties, Inc. | Process for recovery of zirconium basic sulfate |
| CN1367136A (en) * | 2002-02-28 | 2002-09-04 | 柳云珍 | Production process of tetrahydrated zirconium sulfate |
| CN107840363A (en) * | 2017-12-23 | 2018-03-27 | 淄博广通化工有限责任公司 | Environment-friendly inexpensive industrial carbonic acid zirconium production method |
| CN108128804A (en) * | 2017-12-23 | 2018-06-08 | 淄博广通化工有限责任公司 | Industrial carbonic acid zirconium of the good stable storing of purity high activity and preparation method thereof |
-
2020
- 2020-03-06 CN CN202010149298.8A patent/CN111204803A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1316107A (en) * | 1918-07-15 | 1919-09-16 | Pennsylvania Salt Mfg Co | Basic sulfate of zirconium and method of making the same. |
| GB606681A (en) * | 1944-05-11 | 1948-08-18 | Produits Chim Terres Rares Soc | An improved method for obtaining industrially pure double sodium zirconium sulphates |
| US5470550A (en) * | 1993-12-30 | 1995-11-28 | Westinghouse Electric Corporation | Zirconium sulfate precipitation |
| US6358484B1 (en) * | 2000-03-31 | 2002-03-19 | Ati Properties, Inc. | Process for recovery of zirconium basic sulfate |
| CN1367136A (en) * | 2002-02-28 | 2002-09-04 | 柳云珍 | Production process of tetrahydrated zirconium sulfate |
| CN107840363A (en) * | 2017-12-23 | 2018-03-27 | 淄博广通化工有限责任公司 | Environment-friendly inexpensive industrial carbonic acid zirconium production method |
| CN108128804A (en) * | 2017-12-23 | 2018-06-08 | 淄博广通化工有限责任公司 | Industrial carbonic acid zirconium of the good stable storing of purity high activity and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| RACHID ISSAADI ET AL.: "Palladium–sulfated zirconium pillared montmorillonite:Catalytic evaluation in light naphtha hydroisomerization reaction", 《CATALYSIS TODAY》 * |
| 蒋东民: "《氧氯化锆制备工艺与应用 2012年8月第1版》", 31 August 2012, 冶金工业出版社 * |
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