CN101665267A - Preparation method of anhydrous stannous chloride - Google Patents
Preparation method of anhydrous stannous chloride Download PDFInfo
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- CN101665267A CN101665267A CN200910094790A CN200910094790A CN101665267A CN 101665267 A CN101665267 A CN 101665267A CN 200910094790 A CN200910094790 A CN 200910094790A CN 200910094790 A CN200910094790 A CN 200910094790A CN 101665267 A CN101665267 A CN 101665267A
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- drying
- stannous chloride
- anhydrous stannous
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Abstract
The invention relates to a preparation method of anhydrous stannous chloride, in particular to a large-scale production method of anhydrous stannous chloride, belonging to the technical field of the chemical engineer. The method of the invention is to use SnCl2.2H2O as raw material to perform two-stage drying, wherein in the first stage, the first stage drying is performed at normal pressure whilethe heating temperature is controlled to less than 130 DEG C, then organic dispersant is added, the second stage drying adopts vacuum drying, the drying temperature is controlled to 90-110 DEG C andthe vacuum degree is controlled to less than 0.075MPa. The invention has simple process flow and high product purity and is easy to control; and the method can use common chemical equipment and effectively solve the problem of equipment corrosion. The main content of the product prepared by the method is not less than 99% and the solution obtained by dissolving the product in hydrochloric acid solution is clear.
Description
Technical field
The present invention relates to a kind of manufacture method of inorganic tin compound, concrete a kind of method that relates to the large-scale production of anhydrous stannous chloride belongs to chemical technology field.
Background technology
Tin protochloride has anhydrous and contains two kinds of forms of two crystal water, and crystallization tin protochloride fusing point is low, under 37.7 ℃, just be dissolved in the crystal water of self, and easily oxidation, and anhydrous stannous chloride quite stable in air, its purposes is extensive far beyond the crystallization tin protochloride.There is very strong reductibility the anhydrous chlorides of rase Asia, is widely used as reductive agent, uses in inorganic and organic compound manufacturing, printing and dyeing industry, is widely used in wicking process and alloy plating.According to pertinent data, the production method of anhydrous stannous chloride has following several usually:
(1) uses SnCl
22H
2The dehydration of O direct heating;
(2) heating tin or stannous sulfide in the exsiccant hydrogen chloride gas;
(3) use SnCl
22H
2O mixes with dewatering agent, isolates anhydride, and uses detergent washing, and filtration drying makes anhydride then;
(4) reduce anhydrous stannic chloride (SnCl with metallic tin
4).
Above method now only is confined to laboratory preparation, can not solve problems such as the equipment corrosion that enlarges in producing and environmental pollution, and the production cost height.
Summary of the invention
The object of the present invention is to provide a kind of manufacture method of anhydrous stannous chloride scale production, its technical process is simple, is easy to control, and the product purity height can utilize common chemical industry equipment, has effectively solved the problem of equipment corrosion.
Realize that the technical scheme that above-mentioned purpose of the present invention adopted is: with SnCl
22H
2O is a raw material, divides two sections and carries out drying, and first section normal pressure controlled the heating thickening temperature down less than 130 ℃, adds organic dispersing agent, and second section drying carried out vacuum-drying to material, and the control drying temperature is 90～110 ℃, and vacuum tightness is lower than 0.075MPa.
First section constant pressure and dry of the present invention adopts steam heating, 9%～11% moisture content should be removed, and the organic dispersing agent of adding is a H-3 type aluminate coupling agent, and add-on is 0.2 ‰ of raw material weight～0.4 ‰.
The second vacuum-drying period of the present invention is 3h～4h.
The temperature that will control in first section constant pressure and dry process in the concentrating pan can not surpass 130 ℃, can prevent that temperature is too high, Sn
2+Ion is oxidized, finally causes the outward appearance jaundice of product, and a large amount of moisture content and acid gas is being removed in one section material when dry, avoided two sections vacuum drying ovens corrosion.When material is sloughed a part of water, stop heating, add organic dispersing agent, after continuing to stir for some time, material is carried out two-stage vacuum-drying dehydration.The adding of organic dispersing agent can reduce SnCl
2Intermolecular Fan Dehuali and static bonding force make the finished product broken easily, and prevent to lump again after packaged product from placing for some time.
The present invention compared with prior art has the following advantages:
1, technical feasibility, technology is reasonable, and method is simple, and is easy to operate, and the processing parameter of determining can stably be realized suitability for industrialized production.
2, this technical process is simple, is easy to control, the product purity height, and straight, time rate height adopts conventional chemical industry equipment, and production cost is low, no waste discharge.
Embodiment
Embodiment one
Take by weighing 1kg two water crystallization tin protochlorides in beaker, place on the electric furnace and heat, carry out one section concentrate drying.After the material in the beaker has a large amount of white crystals to separate out, stop heating, the top temperature of this process material is 125 ℃, after material is cooled to 90 ℃, add the 0.4g organic dispersing agent, stir 1min after, material is poured in the porcelain baking tray, put into vacuum drying oven and carry out two sections vacuum-dryings, drying temperature is 105 ℃, vacuum tightness 0.082MPa, when no longer including the tangible globule on the vacuum loft drier visor, stop drying, material is taken out, be cooled to normal temperature, carry out fragmentation, obtain 0.832kg anhydrous stannous chloride product, product master content is 99.18%, be dissolved in hydrochloric acid soln after solution limpid.
Embodiment two
Take by weighing 1.5kg two water crystallization tin protochlorides in beaker, place on the electric furnace and heat, carry out one section concentrate drying.After the material in the beaker has a large amount of white crystals to separate out, stop heating, the top temperature of this process material is 127 ℃, after material is cooled to 90 ℃, add the 0.5g organic dispersing agent, stir 1min after, material is poured in the porcelain baking tray, put into vacuum drying oven and carry out two sections vacuum-dryings, drying temperature is 102 ℃, vacuum tightness 0.082MPa, when no longer including the tangible globule on the vacuum loft drier visor, stop drying, material is taken out, be cooled to normal temperature, carry out fragmentation, obtain 1.250kg anhydrous stannous chloride product, product master content is 99.32%, be dissolved in hydrochloric acid soln after solution limpid.
Embodiment three
Taking by weighing 450kg two water crystallization tin protochlorides puts in the enamel still, logical steam heating, after two water tin protochlorides all melt and come to life, open and stir, carry out one section concentrate drying, begin the adularescent crystallization after being concentrated to a certain degree to separate out, continue heating, add the 110g organic dispersing agent when very thick to material, after continuing to stir 10min, material is put in the groove that connects material, reinstalled the enamel baking tray, put into vacuum drying oven and carry out drying, drying temperature is 98 ℃, and vacuum tightness is 0.078MPa, vacuum breaker behind the dry 3.5h, material is taken out, be cooled to normal temperature, carry out fragmentation, obtain 375kg anhydrous stannous chloride product, product master content is 99.24%, be dissolved in hydrochloric acid soln after solution limpid.
Claims (3)
1, a kind of manufacture method of anhydrous stannous chloride is characterized in that: with SnCl
22H
2O is a raw material, divides two sections and carries out drying, and first section normal pressure controlled the heating thickening temperature down less than 130 ℃, adds organic dispersing agent, and second section drying carried out vacuum-drying to material, and the control drying temperature is 90～110 ℃, and vacuum tightness is lower than 0.075MPa.
2, the manufacture method of anhydrous stannous chloride according to claim 1 is characterized in that: first section constant pressure and dry adopts steam heating, 9%～11% moisture content should be removed.
3, the manufacture method of anhydrous stannous chloride according to claim 1 is characterized in that: the organic dispersing agent of adding is a H-3 type aluminate coupling agent, and add-on is 0.2 ‰ of raw material weight～0.4 ‰, and second vacuum-drying period is 3h～4h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100947903A CN101665267B (en) | 2009-08-03 | 2009-08-03 | Preparation method of anhydrous stannous chloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100947903A CN101665267B (en) | 2009-08-03 | 2009-08-03 | Preparation method of anhydrous stannous chloride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101665267A true CN101665267A (en) | 2010-03-10 |
| CN101665267B CN101665267B (en) | 2011-12-28 |
Family
ID=41802080
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|---|---|---|---|
| CN2009100947903A Active CN101665267B (en) | 2009-08-03 | 2009-08-03 | Preparation method of anhydrous stannous chloride |
Country Status (1)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102942214A (en) * | 2012-10-23 | 2013-02-27 | 上海精胜精细化工科技有限公司 | Method for producing stannous sulfide |
| CN110563029A (en) * | 2019-10-30 | 2019-12-13 | 广东先导稀材股份有限公司 | Stannous chloride dihydrate and preparation method thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2516235B (en) * | 2013-07-15 | 2015-12-30 | William Blythe Ltd | Free flowing stannous chloride |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BE791324A (en) * | 1971-11-16 | 1973-03-01 | Vulcan Materials Co | PREPARATION OF STANNY CHLORIDE |
-
2009
- 2009-08-03 CN CN2009100947903A patent/CN101665267B/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102942214A (en) * | 2012-10-23 | 2013-02-27 | 上海精胜精细化工科技有限公司 | Method for producing stannous sulfide |
| CN110563029A (en) * | 2019-10-30 | 2019-12-13 | 广东先导稀材股份有限公司 | Stannous chloride dihydrate and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN101665267B (en) | 2011-12-28 |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Yunnan Tin Co.,Ltd. Assignor: Yunnan Tin Group (Holding) Co., Ltd Contract record no.: 2012530000028 Denomination of invention: Preparation method of anhydrous stannous chloride Granted publication date: 20111228 License type: Exclusive License Open date: 20100310 Record date: 20120522 |
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| TR01 | Transfer of patent right |
Effective date of registration: 20190626 Address after: 661199 Metallurgical Materials Development Zone, Mengzi Economic and Technological Development Zone, Honghe Hani and Yi Autonomous Prefecture, Yunnan Province Patentee after: Yunnan Tin Industry Tin Chemical Materials Co., Ltd. Address before: 661000 Honghe Technology Park, Datun Town, Gejiu City, Yunnan Province Patentee before: Yunnan Tin Co., Ltd., Chemical Materials Branch |
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| TR01 | Transfer of patent right |