CN101293670A - Method for preparing high purity hydrous zirconium oxide and zircon salt with zirconium oxychloride mother solution - Google Patents
Method for preparing high purity hydrous zirconium oxide and zircon salt with zirconium oxychloride mother solution Download PDFInfo
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- CN101293670A CN101293670A CNA2007100543116A CN200710054311A CN101293670A CN 101293670 A CN101293670 A CN 101293670A CN A2007100543116 A CNA2007100543116 A CN A2007100543116A CN 200710054311 A CN200710054311 A CN 200710054311A CN 101293670 A CN101293670 A CN 101293670A
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Abstract
The invention discloses a method of a mother liquid for preparing hydrous zirconium oxide with high purity and a zirconium salt in the production process of zirconium oxychloride. The invention comprises the processes of concentration, hydrolysis, acid corrosion, secondary concentration, crystallization and acid pickling. The invention employs the mother liquid that produces the zirconium oxychloride as the raw material to produce the hydrous zirconium oxide with the high purity, prepare the high value zirconium salt and recycle hydrochloride in the solution. In the process of removing impurities from the solution, a lot of impurities are removed, which leads the product to have the high purity, stable performance and good quality; the hydrochloride can be used repeatedly, which reduces the production cost; the production process of the invention is simple and convenient and is suitable for large scale industrial production.
Description
Technical field
The invention belongs to chemical technology field, be specifically related to the method that mother liquor in a kind of basic zirconium chloride production process prepares high purity hydrous zirconium oxide and prepares zirconates.
Background technology
Produce a large amount of acidity in the basic zirconium chloride production process and contain the zirconium mother liquor, if return production system, owing to impurity such as the sodium in the mother liquor, titanium, silicon, iron can't be removed, along with the carrying out of production cycle, more and more enrichment brings many-sided unfavorable factor to ordinary production.If with the mother liquor discharging, then cause environmental pollution, the wasting of resources, production cost to increase.Therefore, how rationally to recycle the focus that this part mother liquor becomes numerous enterprises and scientific research department's care.
The method of extensively taking at present is: 1, utilize the spent acid in the mother liquor, itself and zirconate (sodium, calcium) are fully stirred evenly, solid-liquid separation makes the zirconium in the zirconate separate with part sodium or calcium again.2, in acidizing process, mix with concentrated hydrochloric acid and to join, drop in the acidification vessel.The shortcoming of these two kinds of methods is, all brings impurity such as sodium a large amount of in the mother liquor, titanium, silicon, iron into system, and almost can't remove, can only enrichment more causes many-sided unfavorable factor to production along with the circulation of producing; And a large amount of hydrochloric acid is not fully utilized in the mother liquor, causes the waste on the resource.
Summary of the invention
The purpose of invention provides a kind of method of extracting highly purified hydrous zirconium oxide and prepare zirconates from the basic zirconium chloride mother liquor, and reclaims the hydrochloric acid in the mother liquor simultaneously, makes mother liquor obtain the method for the most rational recycling.
The basic zirconium chloride mother liquor prepares the method for high purity hydrous zirconium oxide, may further comprise the steps:
A, will contain ZrO
25～120g/l, HCl10～250g/l and TiO
2, SiO
2, Na
2O, Fe
2O
3Mother liquid evaporation Deng impurity concentrates, and reclaims evaporation dilute hydrochloric acid, reduces the total acid content of mother liquor;
B, will contain the acid mother liquor thin up in the A step, slowly be heated to boiling, in heat-processed, add reductive agent and react, when solution PH is 0.3～2.2, the zirconium white [ZrO in the solution
2] hydrolysis takes place, with hydrous zirconium oxide [ZrO (OH)
2.XH
2O] form precipitation;
C, the resultant in the B step is carried out solid-liquid separation, the metaborate monohydrate zirconium white makes hydrous zirconium oxide separate with impurity such as iron, sodium through water washing, the high purity hydrous zirconium oxide precipitation.
Above-mentioned basic zirconium chloride mother liquor prepares the method for high purity hydrous zirconium oxide, and the reductive agent that adds among the described Bu Sudden B is a kind of in tetrahydrofuran (THF), oxalic acid, oxammonium hydrochloride, the thiourea peroxide.
The reductive agent that adds among the described Bu Sudden of the method B that above-mentioned basic zirconium chloride mother liquor prepares high purity hydrous zirconium oxide is a kind of in metallic aluminium, the magnesium.
The reductive agent that adds among the described Bu Sudden of the method B that above-mentioned basic zirconium chloride mother liquor prepares high purity hydrous zirconium oxide is a kind of in S-WAT, potassium sulfite, the ammonium sulfite.
High purity hydrous zirconium oxide prepares the method for zirconates, may further comprise the steps:
A, with highly purified hydrous zirconium oxide [ZrO (OH)
2.XH
2O] place acidification vessel, drop into strong acid, heated and boiled makes the hydrous zirconium oxide dissolving, generates zirconium salt solution, and wherein zirconium dioxide content is 20～100 grams per liters;
B, the heating of the zirconium salt solution that obtains among the A is concentrated, it is sour to reclaim recyclable evaporation, and free acid 2.5-8.5mol/l to the solution is when zirconium dioxide content is 100～260 grams per liters.
C, zirconates crystal among the B is separated with mother liquor, the zirconates crystal.
Prepare the method for zirconates with high purity hydrous zirconium oxide, drop into strong acid among the described Bu Sudden A and be a kind of in 10%～31% hydrochloric acid, 20-93% sulfuric acid and the 20-68% nitric acid.
The method for preparing zirconates with high purity hydrous zirconium oxide, the described steps A of method that the basic zirconium chloride mother liquor prepares high purity hydrous zirconium oxide of being meant 10%～31% the hydrochloric acid that drops in the described steps A reclaims the dilute hydrochloric acid of evaporation and the described step B of method that high purity hydrous zirconium oxide prepares zirconates reclaims the hydrochloric acid of evaporation, adds concentrated hydrochloric acid and is adjusted to 10%～31% hydrochloric acid.
The method that this basic zirconium chloride mother liquor prepares high purity hydrous zirconium oxide and prepares zirconates has the following advantages:
A. by concentration and evaporation, at first the hydrochloric acid in the mother liquor is reclaimed, be can be used for acidleach, pickling process;
B. at hydrolyzing process, zirconium is precipitated out from the mother liquor that contains a large amount of impurity, with sodium, silicon, etc. impurity effectively separate;
C. this method is not subjected to ZrO in the mother liquor
2The restriction of content is not subjected to what influence of foreign matter content in the mother liquor, regardless of mother liquor composition, all can therefrom zirconium be extracted; And then produce highly purified zirconates product, as the basic zirconium chloride crystal;
D. this method can add hydrochloric acid, sulfuric acid etc. and makes different zirconates
E. this method also can be used as the effective ways that the basic zirconium chloride crystal is purified; Also contain zirconium solution applicable to reclaiming other;
F. this method technology is simple, easy handling, and whole technology is not introduced other materials except adding reductive agent.
Description of drawings
Fig. 1 prepares the process flow sheet of hydrous zirconium oxide for the present invention
Fig. 2 prepares the process flow sheet of basic zirconium chloride for the present invention
Fig. 3 prepares the process flow sheet of zirconium sulfate for the present invention
Fig. 4 prepares the process flow sheet of zirconium nitrate for the present invention
Specific embodiment is as follows
Embodiment 1
Contain ZrO
237.58g/l, HC1 179.58g/l and Ti O
215.04g/l, Fe
2O
320.20g/l, Na
2The mother liquor 2000ml of O18.62g/l impurity places matrass, and heating is concentrated into about 1/3 of original volume.Moisturizing is to 2000ml, constantly adds 30% sodium sulfite aqueous solution in this solution, and slowly heating constantly detects solution with the PH test paper simultaneously, to PH be 1.2 o'clock, stop to add S-WAT, continue to be heated to boiling.Like this, the zirconium ion in the solution precipitates with the form of hydrous zirconium oxide.With the hydrous zirconium oxide sedimentation and filtration, washing, till detecting washing lotion and do not have blue look and occur with 5% potassium ferricyanide solution, illustrate precipitate in contained ferrous ion reach requirement.With 500 milliliter of 25% dissolving with hydrochloric acid hydrous zirconium oxide precipitation, obtain zirconium oxychloride aqueous solution, be concentrated into 400 milliliters by heating, add 250 milliliter of 25% hydrochloric acid then, detect ZrO in the solution
2Content reaches 140 grams per liters, and HCl content reaches 182.5 grams per liters, and this solution is cooled to room temperature, separates, and then obtains basic zirconium chloride crystal 181 grams, 1600 milliliters of the hydrochloric acid of percent crystallization in massecuite 75.3%, twice concentrated recovery 16%.
Embodiment 2
Contain ZrO
237.58g/l, HCl 179.58g/l and a large amount of TiO
215.04g/l, Fe
2O
320.20g/l, Na
2The mother liquor 2000ml of impurity such as O 18.62g/l places matrass, and heating is concentrated into about 1/3 of original volume.Moisturizing is to 2000ml, constantly adds 30% the ammonium sulfite aqueous solution in this solution, and slowly heating constantly detects solution with the PH test paper simultaneously, to PH be 0.9 o'clock, stop to add ammonium sulfite, continue to be heated to boiling.Like this, the zirconium ion in the solution precipitates with the form of hydrous zirconium oxide.With the hydrous zirconium oxide sedimentation and filtration, washing, till detecting washing lotion and do not have blue look and occur with 5% potassium ferricyanide solution, illustrate precipitate in contained ferrous ion reach requirement.With 500 milliliter of 25% dissolving with hydrochloric acid hydrous zirconium oxide precipitation, obtain zirconium oxychloride aqueous solution, be concentrated into 400 milliliters by heating, add 250 milliliter of 25% hydrochloric acid then, detect ZrO in the solution
2Content reaches 140 grams per liters, and HCl content reaches 182.5 grams per liters, and this solution is cooled to room temperature, separates, and then obtains basic zirconium chloride crystal 179 grams, 1500 milliliters of the hydrochloric acid of percent crystallization in massecuite 74.9%, twice concentrated recovery 16%.
Embodiment 3
Contain ZrO
237.58g/l, HCl 179.58g/l and a large amount of Ti O
215.04g/l, Fe
2O
320.20g/l, Na
2The mother liquor 2000ml of impurity such as O18.62g/l places matrass, and heating is concentrated into about 1/3 of original volume.Moisturizing is to 2000ml, constantly adds 30% the potassium sulfite aqueous solution in this solution, and slowly heating constantly detects solution with the PH test paper simultaneously, to PH be 1.2 o'clock, stop to add potassium sulfite, continue to be heated to boiling.Like this, the zirconium ion in the solution precipitates with the form of hydrous zirconium oxide.With the hydrous zirconium oxide sedimentation and filtration, washing, till detecting washing lotion and do not have blue look and occur with 5% potassium ferricyanide solution, illustrate precipitate in contained ferrous ion reach requirement.With 500 milliliter of 25% dissolving with hydrochloric acid hydrous zirconium oxide precipitation, obtain zirconium oxychloride aqueous solution, be concentrated into 400 milliliters by heating, add 250 milliliter of 25% hydrochloric acid then, detect ZrO in the solution
2Content reaches 140 grams per liters, and HCl content reaches 182.5 grams per liters, and this solution is cooled to room temperature, separates, and then obtains basic zirconium chloride crystal 184 grams, 1600 milliliters of the hydrochloric acid of percent crystallization in massecuite 75.2%, twice concentrated recovery 16%.
Embodiment 4
Contain ZrO
237.58g/l, HCl 179.58g/l and a large amount of TiO
215.04g/l, Fe
2O
320.20g/l, Na
2The mother liquor 2000ml of impurity such as O18.62g/l places matrass, and heating is concentrated into about 1/3 of original volume.Moisturizing is to 2000ml, constantly adds 30% sodium sulfite aqueous solution in this solution, and slowly heating constantly detects solution with the PH test paper simultaneously, to PH be 1.0 o'clock, stop to add S-WAT, continue to be heated to boiling.Like this, the zirconium ion in the solution precipitates with the form of hydrous zirconium oxide.With the hydrous zirconium oxide sedimentation and filtration, washing, till detecting washing lotion and do not have blue look and occur with 5% potassium ferricyanide solution, illustrate precipitate in contained ferrous ion reach requirement.With 500 milliliter of 25% dissolving with hydrochloric acid hydrous zirconium oxide precipitation, obtain zirconium oxychloride aqueous solution, be concentrated into 400 milliliters by heating, add 250 milliliter of 25% hydrochloric acid then, ZrO in solution
2Content reaches 140 grams per liters, and HCl content reaches 182.5 grams per liters, and this solution is cooled to room temperature, separates, and then obtains basic zirconium chloride crystal 183 grams, 1600 milliliters of the hydrochloric acid of percent crystallization in massecuite 74.3%, twice concentrated recovery 16%.
Embodiment 5
Contain ZrO
237.58g/l, HCl 179.58g/l and a large amount of TiO
215.04g/l, Fe
2O
320.20g/l, Na
2The mother liquor 2000ml of impurity such as O18.62g/l places matrass, and heating is concentrated into about 1/3 of original volume.Moisturizing constantly adds 30% sodium sulfite aqueous solution to 2000ml in this solution, slowly heating to PH=1.8, stops to add S-WAT simultaneously, continues to be heated to boiling.Like this, the zirconium ion in the solution precipitates with the form of hydrous zirconium oxide.With the hydrous zirconium oxide sedimentation and filtration, washing, till detecting washing lotion and do not have blue look and occur with 5% potassium ferricyanide solution, illustrate precipitate in contained ferrous ion reach requirement.With 500 milliliter of 25% dissolving with hydrochloric acid hydrous zirconium oxide precipitation, obtain zirconium oxychloride aqueous solution, be concentrated into 400 milliliters by heating, add 250 milliliter of 25% hydrochloric acid then, detect ZrO in the solution
2Content reaches 130 grams per liters, and HCl content reaches 182.5 grams per liters, and this solution is cooled to room temperature, separates, and then obtains basic zirconium chloride crystal 170 grams, 1600 milliliters of the hydrochloric acid of percent crystallization in massecuite 75.1%, twice concentrated recovery 16%.
In the above-mentioned preparation basic zirconium chloride step, ZrO in the mother liquor
2Can also take off numerical value in the table with zirconium white and HCl in HCL concentration, the crystallisation by cooling step in reductive agent and pH value, the step of acid dipping in the content of, HCl, the hydrolytic process
5 embodiment basic zirconium chloride product detected results see the following form:
Embodiment 6
Contain ZrO
237.58g/l, HCl 179.58g/l and a large amount of TiO
215.04g/l, Fe
2O
320.20g/l, Na
2The mother liquor 2000ml of impurity such as O18.62g/l places matrass, and heating is concentrated into about 1/3 of original volume.Moisturizing constantly adds 30% sodium sulfite aqueous solution to 2000ml in this solution, slowly heating to PH=1.2, stops to add S-WAT simultaneously, continues to be heated to boiling.Like this, the zirconium ion in the solution precipitates with the form of hydrous zirconium oxide.With the hydrous zirconium oxide sedimentation and filtration, washing, till detecting washing lotion and do not have blue look and occur with 5% potassium ferricyanide solution, illustrate precipitate in contained ferrous ion reach requirement.With 200 milliliter of 50% sulfuric acid dissolution hydrous zirconium oxide precipitation, heating concentrates ZrO in solution then
2Content 140g/l, free sulfuric acid content 5mol/l with this solution crystallisation by cooling, separates, and then obtains the zirconium sulfate crystal.In the above-mentioned preparation zirconium sulfate step, ZrO in the mother liquor
2With H in reductive agent and pH value, the step of acid dipping in the content of, HCl, the hydrolytic process
2SO
4, zirconium white and H in the concentration, crystallisation by cooling step
2SO
4Can also take off numerical value in the table
Embodiment 7
Contain ZrO
237.58g/l, HCl 179.58g/l and a large amount of Ti O
215.04g/l, Fe
2O
320.20g/l, Na
2018.62g/l Deng the mother liquor 2000ml of impurity, place matrass, heating is concentrated into about 1/3 of original volume.Moisturizing constantly adds 30% sodium sulfite aqueous solution to 2000ml in this solution, slowly heating to PH=2.1, stops to add S-WAT simultaneously, continues to be heated to boiling.Like this, the zirconium ion in the solution precipitates with the form of hydrous zirconium oxide.With the hydrous zirconium oxide sedimentation and filtration, washing, till detecting washing lotion and do not have blue look and occur with 5% potassium ferricyanide solution, illustrate precipitate in ferrous ion reach requirement.With 400 milliliter of 55% nitric acid dissolve hydrous zirconium oxide precipitation, heating concentrates ZrO in solution then
2Content reaches 200g/l, and free nitric acid content 7mol/l with this solution crystallisation by cooling, separates, and then obtains the zirconium nitrate crystal.In the above-mentioned preparation zirconium sulfate step, ZrO in the mother liquor
2With HNO in reductive agent and pH value, the step of acid dipping in the content of HCl, the hydrolytic process
3, zirconium white and HNO in the concentration, crystallisation by cooling step
3Can also take off numerical value in the table
Claims (7)
1, basic zirconium chloride (or zirconyl chloride) mother liquor prepares the method for high purity hydrous zirconium oxide, may further comprise the steps:
A, will contain ZrO
25～100g/l, HCl10～250g/l and TiO
2, SiO
2, Na
2O, Fe
2O
3The mother liquid evaporation of impurity concentrates, and reclaims evaporation dilute hydrochloric acid, reduces the total acid content in the mother liquor;
B, will contain the acid mother liquor thin up in the A step, slowly be heated to boiling, in heat-processed, add reductive agent and react, when solution PH is 0.3～2.2, the zirconium white [ZrO in the solution
2] hydrolysis takes place, with hydrous zirconium oxide [ZrO (OH)
2.XH
2O] form precipitation; C, the resultant in the B step is carried out solid-liquid separation, the metaborate monohydrate zirconium white makes hydrous zirconium oxide and SiO through water washing
2, Na
2O, Fe
2O
3Impurity separates, and obtains the high purity hydrous zirconium oxide precipitation.
2, prepare the method for high purity hydrous zirconium oxide according to claim 1 basic zirconium chloride mother liquor, it is characterized in that: the reductive agent that adds among the described Bu Sudden B is a kind of in tetrahydrofuran (THF), oxalic acid, oxammonium hydrochloride, the thiourea peroxide.
3, prepare the method for high purity hydrous zirconium oxide according to claim 1 basic zirconium chloride mother liquor, it is characterized in that: reductive agent is a kind of in metallic aluminium, the magnesium among the described Bu Sudden B.
4, prepare the method for high purity hydrous zirconium oxide according to claim 1 basic zirconium chloride mother liquor, it is characterized in that: reductive agent is a kind of in S-WAT, potassium sulfite, the ammonium sulfite among the described Bu Sudden B.
5, prepare the method that high purity hydrous zirconium oxide prepares zirconates according to claim 1-4 is described, may further comprise the steps:
A, with highly purified hydrous zirconium oxide [ZrO (OH)
2.XH
2O] place acidification vessel, drop into strong acid, heated and boiled makes the hydrous zirconium oxide dissolving, generates zirconium salt solution, and wherein zirconium dioxide content is the 20-100 grams per liter.
B, the heating of the zirconium salt solution that obtains among the A is concentrated, reclaim recyclable acid, free acid content is 2.5～8.5mol/l to the solution, and zirconium dioxide content is 100～260 grams per liters, carries out crystallisation by cooling and generates zirconates crystal and mother liquor;
C, zirconates crystal among the B is separated with mother liquor, the zirconates crystal.
6, according to claim 5ly prepare the method for zirconates, it is characterized in that: drop into a kind of in hydrochloric acid, 20-93% sulfuric acid and the 20-68% nitric acid that strong acid is 10%-31% among the described Bu Sudden A with high purity hydrous zirconium oxide.
7, according to claim 5 or the 6 described methods that prepare zirconates with high purity hydrous zirconium oxide, it is characterized in that: 10%～31% the hydrochloric acid that drops in the described steps A is meant that the described steps A of method that the basic zirconium chloride mother liquor prepares high purity hydrous zirconium oxide reclaims the dilute hydrochloric acid of evaporation and the described step B of method that high purity hydrous zirconium oxide prepares zirconates reclaims the hydrochloric acid of evaporation, adds concentrated hydrochloric acid and is adjusted to 10%～31% hydrochloric acid.
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|---|---|---|---|
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102776803A (en) * | 2012-04-20 | 2012-11-14 | 深圳市瑞成科讯实业有限公司 | Preparation method for preparing potassium-zirconium-carbonate water repellent agent |
| CN103086427A (en) * | 2013-02-21 | 2013-05-08 | 江苏九九久科技股份有限公司 | Method for preparing nano zirconium dioxide powder by vacuum variable-pressure acid distillation dechlorination |
| CN103174059A (en) * | 2013-03-14 | 2013-06-26 | 河南工业大学 | Method for producing silicon particle pulp as retention aid for papermaking by using zirconium oxychloride discharge waste residue liquid |
| CN111204801A (en) * | 2020-01-21 | 2020-05-29 | 绵竹市金坤化工有限公司 | Phosphoric acid method production process of zirconia powder of high-silicon zirconium-containing waste |
| CN115448362A (en) * | 2022-08-29 | 2022-12-09 | 焦天棋 | Method for separating and preparing zirconium salt and preparing zirconium oxide solid from zirconium oxychloride mother liquor |
-
2007
- 2007-04-27 CN CNA2007100543116A patent/CN101293670A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102776803A (en) * | 2012-04-20 | 2012-11-14 | 深圳市瑞成科讯实业有限公司 | Preparation method for preparing potassium-zirconium-carbonate water repellent agent |
| CN103086427A (en) * | 2013-02-21 | 2013-05-08 | 江苏九九久科技股份有限公司 | Method for preparing nano zirconium dioxide powder by vacuum variable-pressure acid distillation dechlorination |
| CN103086427B (en) * | 2013-02-21 | 2014-06-25 | 江苏九九久科技股份有限公司 | Method for preparing nano zirconium dioxide powder by vacuum variable-pressure acid distillation dechlorination |
| CN103174059A (en) * | 2013-03-14 | 2013-06-26 | 河南工业大学 | Method for producing silicon particle pulp as retention aid for papermaking by using zirconium oxychloride discharge waste residue liquid |
| CN103174059B (en) * | 2013-03-14 | 2014-11-19 | 河南工业大学 | Method for producing silicon particle pulp as retention aid for papermaking by using zirconium oxychloride discharge waste residue liquid |
| CN111204801A (en) * | 2020-01-21 | 2020-05-29 | 绵竹市金坤化工有限公司 | Phosphoric acid method production process of zirconia powder of high-silicon zirconium-containing waste |
| CN111204801B (en) * | 2020-01-21 | 2022-04-01 | 绵竹市金坤化工有限公司 | Phosphoric acid method production process of zirconia powder of high-silicon zirconium-containing waste |
| CN115448362A (en) * | 2022-08-29 | 2022-12-09 | 焦天棋 | Method for separating and preparing zirconium salt and preparing zirconium oxide solid from zirconium oxychloride mother liquor |
| CN115448362B (en) * | 2022-08-29 | 2024-01-16 | 焦天棋 | Method for separating and preparing zirconium salt from zirconium oxychloride mother solution and preparing zirconium oxide solid |
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