CN105329936B - A kind of preparation method of sodium stannate product of the whiteness more than 95 degree - Google Patents
A kind of preparation method of sodium stannate product of the whiteness more than 95 degree Download PDFInfo
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- CN105329936B CN105329936B CN201510871300.1A CN201510871300A CN105329936B CN 105329936 B CN105329936 B CN 105329936B CN 201510871300 A CN201510871300 A CN 201510871300A CN 105329936 B CN105329936 B CN 105329936B
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Abstract
The present invention discloses a kind of preparation method of sodium stannate product of whiteness more than 95 degree, comprises the following steps：（1）Leach thick sodium stannate：Take thick sodium stannate, NaOH, water heating response；（2）Add NaOH regulation alkali contents；（3）Oxidation：Hydrogen peroxide is slowly added to the solution for having configured, reaction to gravity 1.5g/m3Stop heating；（4）Sedimentation：Solution to solid-liquid is stood substantially to be layered；（5）Secondary settlement：Supernatant is taken out into standing sedimentation；（6）Filtering：Supernatant to filter disc is extracted, hydrogen peroxide and circulating filtration is added；（7）Condensing crystallizing：Solution after filtering is concentrated in vacuo, when gravity reaches 1.7g/m3When stop concentration；（8）Separation of solid and liquid；（9）Drying obtains sodium stannate product of the whiteness more than 95 degree.The present invention improves sodium stannate product whiteness by leaching oxidation, filtering oxidation, drying oxidation, can prepare the sodium stannate product that whiteness is more than 95 degree, effective to increase cognition degree of the client to product.
Description
Technical field
The invention belongs to sodium stannate product preparation field, the preparation of sodium stannate product of particularly a kind of whiteness more than 95 degree
Method.
Background technology
Sodium stannate（Sodium stannate）, No. CAS is 12058-66-1, and molecular formula is Na2SnO3, it is colourless hexagonal plate
Shape is crystallized or white powder, tasteless, is insoluble in organic matter, soluble in water, and the aqueous solution is in alkalescence.Sodium stannate is widely used, is used for
The industry such as dyestuff, spices, mirror processed, plating；And as super-pressure lubricating oil, bleaching agent, as reducing agent, mordant, decolorising agent
And analytical reagent, for silver, arsenic, molybdenum, mercury measure.
At present, at 85~90 degree, product appearance carries light gray to the sodium stannate product whiteness of in the market, with sale city
Field saturation, sodium stannate production marketing dog-eat-dog.Outside price factor, product appearance turns into main competition factor.At present not
See sodium stannate production marketing of the whiteness more than 95 degree, also the not disclosed correlation technique for being improved sodium stannate product whiteness.
The content of the invention
The invention aims to overcome the deficiencies in the prior art, there is provided a kind of sodium stannate product of whiteness more than 95 degree
Preparation method, the present invention improve sodium stannate by multiple method for oxidation by leaching oxidation, filtering oxidation, drying oxidation
Product whiteness.
To achieve these goals, the present invention is achieved by the following technical solutions：A kind of tin of whiteness more than 95 degree
The preparation method of sour sodium product, comprises the following steps：
（1）Leach thick sodium stannate：A certain amount of thick sodium stannate is taken, NaOH, water heating response is allocated into, reaction temperature keeps 50~
70 DEG C, thick sodium stannate, NaOH, the mass ratio of water are 1:1:8；
（2）Regulation alkali content：NaOH is added, regulation alkali content is 45~55g/L；
（3）Oxidation：The hydrogen peroxide of concentration 30% is slowly added to the solution for having configured, the addition of 30% hydrogen peroxide is step
（2）The 2%~6% of the liquor capacity for obtaining, reaction to gravity reaches 1.45~1.55g/m3Stop heating；
（4）Sedimentation：Solution to solid-liquid is stood substantially to be layered；
（5）Secondary settlement：By step（4）The supernatant for obtaining is taken out in another container to stand and settles 5~7h again；
（6）Filtering：Extraction step（5）The supernatant for obtaining adds step to filter disc（5）The supernatant volume 5% for obtaining~
11% hydrogen peroxide of concentration 30% and circulating filtration；
（7）Condensing crystallizing：Solution after filtering is carried out into Concentrated and crystallized in vacuum, when gravity reaches 1.65~1.75g/
m3For terminal stops concentrating；
（8）Separation of solid and liquid：Sodium stannate crystal solution after condensing crystallizing is centrifuged, solid sodium stannate is isolated wet
Material；（9）Drying：The drying of solid sodium stannate wet stock is sodium stannate product of the whiteness more than 95 degree.
Further technical scheme of the invention is：Step（4）The sedimentation time of solution left standstill is 22~26h.
Described filter disc filter cloth model 747B, bilayer superposition.
Step（1）Stanniferous amount is 50~55% in thick sodium stannate.
Step（3）Hydrogen peroxide is slowly added to for the range estimation inviolent bubbling of reaction is defined.
Step（9）Drying temperature be 500~550 DEG C, drying time be 2~4 hours.
Compared with prior art, the beneficial effects of the invention are as follows：The present invention is by fully oxidized sodium stannate preparation process
Sn2+、As2+、Sb2+、Pb2+Deng essential element, sodium stannate product whiteness is improved, stannic acid of the whiteness more than 95 degree can be prepared
Sodium product, the effective cognition degree for increasing client to product.
Specific embodiment
With reference to embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to
The scope that embodiment is represented.
Embodiment 1：
The thick sodium stannate material that stanniferous amount is 52% is taken into 200kg and is put into 2m 3Reactive tank in, add 200kgNaOH, plus
Enter 1.6m3Water, is heated to 65 DEG C and keeps, and it is 50g/L to add NaOH regulation alkali contents, is slowly added to the hydrogen peroxide of 8L concentration 30%,
Account for overall solution volume 5%.Question response gravity reaches 1.5g/m3Stop heating.Standing sedimentation 24 hours to solid-liquid substantially divides
Layer, standing carries out secondary settlement 6 hours in extracting supernatant to another container.Secondary settlement supernatant to filter disc is extracted, is added
16L hydrogen peroxide accounts for supernatant cumulative volume 10% and circulating filtration.Solution after filtering is squeezed into concentration tank and is concentrated in vacuo
Crystallization, when gravity reaches 1.7g/m3When stop concentration.Extract condensing crystallizing liquid and be put into centrifuge, be centrifuged, point
Wet stock after is placed in high temperature drying oven, is dried 3 hours, and temperature is kept for 525 DEG C.Blowing is to obtain whiteness more than 95 degree
Sodium stannate product.Produced sodium stannate product chemical examination, measurement result such as table 1.
Embodiment 2：
The thick sodium stannate material that stanniferous amount is 52% is taken into 200kg and is put into 2m 3Reactive tank in, add 200kgNaOH, plus
Enter 1.6m3Water, is heated to 65 DEG C and keeps, and it is 50g/ L to add NaOH regulation alkali contents, is slowly added to the dioxygen of 4L concentration 30%
Water, accounts for overall solution volume 2%.Question response gravity reaches 1.5g/m3Stop heating.Standing sedimentation 24 hours is bright to solid-liquid
Aobvious layering, standing carries out secondary settlement 6 hours in extracting supernatant to another container.Secondary settlement supernatant is extracted to filter disc,
10L hydrogen peroxide is added to account for supernatant cumulative volume 5% and circulating filtration.Solution after filtering is squeezed into carries out vacuum in concentration tank
Condensing crystallizing, when gravity reaches 1.7g/m3When stop concentration.Extract condensing crystallizing liquid and be put into centrifuge, carry out centrifugation point
From the wet stock after separation is placed in high temperature drying oven, is dried 3 hours, and temperature is kept for 525 DEG C.Produced sodium stannate product
Chemical examination, measurement result such as table 2.
Contrast experiment's example 1：
The thick sodium stannate material that stanniferous amount is 52% is taken into 200kg and is put into 2m 3Reactive tank in, add 200kgNaOH, plus
Enter 1.6m3Water, is heated to 65 DEG C and keeps, and it is 50g/ L to add NaOH regulation alkali contents, is added without hydrogen peroxide.Question response solution
Proportion reaches 1.5 g/m3Stop heating.Standing sedimentation is substantially layered for 24 hours to solid-liquid, and extraction supernatant standing carries out secondary
Sedimentation 6 hours.Secondary settlement supernatant is extracted to filter disc, hydrogen peroxide, circulating filtration is added without.Solution after filtering is squeezed into dense
Concentrated and crystallized in vacuum is carried out in contracting tank, when gravity reaches 1.7g/m3When stop concentration.Extract condensing crystallizing liquid and be put into centrifugation
Machine, is centrifuged, and the wet stock after separation is placed in high temperature drying oven, is dried 3 hours, and temperature is kept for 525 DEG C.It is made
Go out the chemical examination of sodium stannate product, measurement result such as table 3.
The product of the NaOH that the present invention is used preferably commercially available main composition >=95.00% of NaOH.The present invention leaches thick
The water of sodium stannate preferably uses sand filter water, the preferred model 747B of filter disc filter cloth, bilayer superposition.It is range estimation to be slowly added to hydrogen peroxide
The inviolent bubbling of reaction is defined.
Sodium stannate product whiteness of the present invention is determined with GB/T 23774-2009 as standard.
Claims (5)
1. a kind of whiteness is more than the preparation method of 95 degree of sodium stannate product, it is characterised in that：Comprise the following steps：
（1）Leach thick sodium stannate：A certain amount of thick sodium stannate is taken, NaOH, water heating response is allocated into, reaction temperature keeps 50~70
DEG C, thick sodium stannate, NaOH, the mass ratio of water are 1:1:8；Stanniferous amount is 50~55% in thick sodium stannate；
（2）Regulation alkali content：NaOH is added, regulation alkali content is 45~55g/L；
（3）Oxidation：The hydrogen peroxide of concentration 30% is slowly added to the solution for having configured, the addition of 30% hydrogen peroxide is step（2）
The 2%~6% of the liquor capacity for obtaining, reaction to gravity reaches 1.45~1.55g/m3Stop heating；
（4）Sedimentation：Solution to solid-liquid is stood substantially to be layered；
（5）Secondary settlement：By step（4）The supernatant for obtaining is taken out in another container to stand and settles 5~7h again；
（6）Filtering：Extraction step（5）The supernatant for obtaining adds step to filter disc（5）The supernatant volume 5%~11% for obtaining
The hydrogen peroxide of concentration 30% and circulating filtration；
（7）Condensing crystallizing：Solution after filtering is carried out into Concentrated and crystallized in vacuum, when gravity reaches 1.65~1.75g/m3For
Terminal stops concentration；
（8）Separation of solid and liquid：Sodium stannate crystal solution after condensing crystallizing is centrifuged, the wet thing of solid sodium stannate is isolated
Material；（9）Drying：The drying of solid sodium stannate wet stock is sodium stannate product of the whiteness more than 95 degree.
2. a kind of whiteness according to claim 1 is more than the preparation method of 95 degree of sodium stannate product, it is characterised in that：Step
Suddenly（4）The sedimentation time of solution left standstill is 22~26h.
3. a kind of whiteness according to claim 1 is more than the preparation method of 95 degree of sodium stannate product, it is characterised in that：Filter
Disk filter cloth model 747B, bilayer superposition.
4. a kind of whiteness according to claim 1 is more than the preparation method of 95 degree of sodium stannate product, it is characterised in that：Step
Suddenly（3）Hydrogen peroxide is slowly added to for the range estimation inviolent bubbling of reaction is defined.
5. a kind of whiteness according to claim 1 is more than the preparation method of 95 degree of sodium stannate product, it is characterised in that：Step
Suddenly（9）Drying temperature be 500~550 DEG C, drying time be 2~4 hours.
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| CN112573565A (en) * | 2020-12-10 | 2021-03-30 | 广东臻鼎环境科技有限公司 | Method for preparing potassium stannate trihydrate by using tin stripping waste liquid |
| CN112456545A (en) * | 2020-12-10 | 2021-03-09 | 广东臻鼎环境科技有限公司 | Method for preparing sodium stannate trihydrate by using tin stripping waste liquid |
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| CN85104036B (en) * | 1985-05-23 | 1987-02-18 | 广东工学院 | Direct prepn. of sodium stannate from tin concentrate |
| CN1078444A (en) * | 1993-06-22 | 1993-11-17 | 郑铁锋 | The preparation method of alkali metal stannate |
| JP4276322B2 (en) * | 1999-02-08 | 2009-06-10 | 日本化学産業株式会社 | Method for producing high purity alkali stannate compound |
| CN101497458B (en) * | 2008-01-30 | 2010-10-06 | 深圳市东江环保股份有限公司 | Method for preparing sodium stannate using circuit board tin-stripping wastewater |
| CN102173448A (en) * | 2011-02-26 | 2011-09-07 | 西陇化工股份有限公司 | Method for preparing alkali metal stannate |
| CN102863015A (en) * | 2012-08-30 | 2013-01-09 | 云南锡业股份有限公司 | Method for preparing sodium stannate |
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Effective date of registration: 20200325 Address after: 547000 No.71, Chengxi Road, Hechi City, Guangxi Zhuang Autonomous Region Patentee after: GUANGXI HUAXI GROUP Co.,Ltd. Address before: 545026 the Guangxi Zhuang Autonomous Region Liuzhou Liu Dong New Area Bay Road No. 2 East standard workshop No. 2 supporting office building No. 314 Patentee before: LIUZHOU BAIRENTE ADVANCED MATERIALS Co.,Ltd. |