CN103934462A - Method for preparing special tin raw material for methyl tin mercaptide - Google Patents
Method for preparing special tin raw material for methyl tin mercaptide Download PDFInfo
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- CN103934462A CN103934462A CN201410216580.8A CN201410216580A CN103934462A CN 103934462 A CN103934462 A CN 103934462A CN 201410216580 A CN201410216580 A CN 201410216580A CN 103934462 A CN103934462 A CN 103934462A
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- tin
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- thiol methyl
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Abstract
The invention provides a method for preparing a special tin raw material for methyl tin mercaptide, belongs to the field of inorganic tin chemical engineering, and particularly relates to the method for preparing the special tin raw material for alkylation reactions of the methyl tin mercaptide. The method includes the steps that a metal tin raw material is placed in a container, heated and molten, so that tin molten liquid passes a diameter-variable pipeline gradually narrowing, meanwhile, water with the pressure ranging from 0.05 MPa to 0.5 MPa is sprayed to the tin molten liquid passing through the diameter-variable pipeline to obtain scale-shaped tin, and then the special tin raw material is obtained after the scale-shaped tin is dried. The specific area of the tin raw material prepared in the method is proper, the surface can not be oxidized, the reactions are easy to control, the raw material is suitable for the alkylation reactions of the methyl tin mercaptide, the tin reacts stably in the alkylation reaction process, and the reactions are complete.
Description
Technical field
The invention belongs to inorganic tin chemical field, be specifically related to a kind of preparation method of the tin raw material that is specifically designed to thiol methyl tin alkylated reaction.
Technical background
The special tin raw material of thiol methyl tin is mainly used in thiol methyl tin alkylated reaction.In thiol methyl tin alkylation process, tin is as key reaction raw material, and the indices that it participates in the tin of reaction, directly affects the speed degree of reaction speed, the safe coefficient of reaction, and then affect production efficiency and business efficiency.For example, if it is too small to participate in the physical form of the tin reacting, during as powdery, abnormal reaction fierceness, can not control; If it is excessive to participate in the physical aspect of the tin reacting, during as fritter shape, sluggish, reaction is not exclusively.The special tin raw material of thiol methyl tin is researched and developed production just in order to solve problems.By controlling tin coolant-temperature gage and water expulsion pressure, can prepare and both can finely carry out alkylated reaction, the special tin raw material of thiol methyl tin that can make alkylated reaction carry out completely again.
Summary of the invention
The object of this invention is to provide the preparation method of the special tin raw material of a kind of thiol methyl tin, the tin raw material of preparing with the method is suitable in thiol methyl tin alkylated reaction, makes tin stable reaction in alkylation process, reacts completely.
Realizing the technical scheme that the object of the invention takes is: metallic tin raw material is inserted to vessel in heating fusing, make tin melt by the tapered pipeline diminishing gradually, water taking pressure as 0.05～0.5MPa sprays the tin melt that has passed through tapered pipeline simultaneously, obtain the tin of fish scale sheet, then can obtain special tin raw material product after dry.
The heavy caliber end diameter of described tapered pipeline is 60～100mm, and small-caliber end diameter is 20～60mm, and length is 60～85mm.
Temperature when described injection tin melt is 235～300 DEG C, nozzle bore 0.5～2.5mm, pitch-row 5～20mm.
It is 100～150 DEG C to the baking temperature that sprays the flakey tin forming.
Useful technique effect of the present invention is: adopt the special tin raw material that obtains of the present invention reaction speed and complete degree of reaction in thiol methyl tin alkylation process to be better than the tin of other forms.Flakey tin and other shape tin are carried out to 10 tests at thiol methyl tin alkylated reaction, and average response completeness is as following table:
。
Brief description of the drawings
Fig. 1 is process chart of the present invention.
Detailed description of the invention
Embodiment 1: add 1.5 tons of tin slabs in the pot of fusing tin, open heater, after the tin in pot is melted, insulation is at 235 DEG C; Start water jet device, adjusting pressure is 0.25MPa; Open above-mentioned tin liquor circulation tapered pipeline, prepare the special tin raw material of thiol methyl tin; After overanxious, proceed in drying equipment, it is 105 DEG C that baking temperature is set, and is dried after 265 minutes, stop being dried, and cooling rear sample examination, water content 0.045% is qualified.
Embodiment 2: add 1.8 tons of tin slabs in the pot of fusing tin, open heater, after the tin in pot is melted, insulation is at 252 DEG C; Start water jet device, adjusting pressure is 0.28MPa; Open above-mentioned tin liquor circulation tapered pipeline, prepare the special tin raw material of thiol methyl tin; After overanxious, proceed in drying equipment, it is 125 DEG C that baking temperature is set, and is dried after 270 minutes, stop being dried, and cooling rear sample examination, water content 0.046% is qualified.
Embodiment 3: add 2 tons of tin slabs in the pot of fusing tin, open heater, after the tin in pot is melted, insulation is at 258 DEG C; Start water jet device, adjusting pressure is 0.28MPa; Open above-mentioned tin liquor circulation tapered pipeline, prepare the special tin raw material of thiol methyl tin; After overanxious, proceed in drying equipment, it is 135 DEG C that baking temperature is set, and is dried after 270 minutes, stop being dried, and cooling rear sample examination, water content 0.045% is qualified.
Embodiment 4: add 2.2 tons of tin slabs in the pot of fusing tin, open heater, after the tin in pot is melted, insulation is at 270 DEG C; Start water jet device, adjusting pressure is 0.28MPa; Open above-mentioned tin liquor circulation tapered pipeline, prepare the special tin raw material of thiol methyl tin; After overanxious, proceed in drying equipment, it is 150 DEG C that baking temperature is set, and is dried after 265 minutes, stop being dried, and cooling rear sample examination, water content 0.05% is qualified.
Embodiment 5: add 2.4 tons of tin slabs in the pot of fusing tin, open heater, after the tin in pot is melted, insulation is at 260 DEG C; Start water jet device, adjusting pressure is 0.1MPa; Open above-mentioned tin liquor circulation tapered pipeline, prepare the special tin raw material of thiol methyl tin; After overanxious, proceed in drying equipment, it is 145 DEG C that baking temperature is set, and is dried after 268 minutes, stop being dried, and cooling rear sample examination, water content 0.045% is qualified.
Embodiment 6: add 2.5 tons of tin slabs in the pot of fusing tin, open heater, after the tin in pot is melted, insulation is at 292 DEG C; Start water jet device, adjusting pressure is 0.28MPa; Open above-mentioned tin liquor circulation tapered pipeline, prepare the special tin raw material of thiol methyl tin; After overanxious, proceed in drying equipment, it is 135 DEG C that baking temperature is set, and is dried after 265 minutes, stop being dried, and cooling rear sample examination, water content 0.045% is qualified.
Claims (4)
1. the preparation method of the special tin raw material of thiol methyl tin, it is characterized in that: metallic tin raw material is inserted to vessel in heating fusing, make tin melt by the tapered pipeline diminishing gradually, water taking pressure as 0.05～0.5MPa sprays the tin melt that has passed through tapered pipeline simultaneously, obtain the tin of fish scale sheet, then can obtain special tin raw material product after dry.
2. by claim
1the preparation method of the described special tin raw material of thiol methyl tin, is characterized in that: the heavy caliber end diameter of tapered pipeline is 60～100mm, and small-caliber end diameter is 20～60mm, and length is 60～85mm.
3. by claim
1the preparation method of the described special tin raw material of thiol methyl tin, is characterized in that: the temperature while spraying tin melt is 235～300 DEG C, nozzle bore 0.5～2.5mm, pitch-row 5～20mm.
4. by claim
1the preparation method of the described special tin raw material of thiol methyl tin, is characterized in that: be 100～150 DEG C to the baking temperature that sprays the flakey tin forming.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410216580.8A CN103934462A (en) | 2014-05-22 | 2014-05-22 | Method for preparing special tin raw material for methyl tin mercaptide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410216580.8A CN103934462A (en) | 2014-05-22 | 2014-05-22 | Method for preparing special tin raw material for methyl tin mercaptide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103934462A true CN103934462A (en) | 2014-07-23 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410216580.8A Pending CN103934462A (en) | 2014-05-22 | 2014-05-22 | Method for preparing special tin raw material for methyl tin mercaptide |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH024906A (en) * | 1988-06-22 | 1990-01-09 | Takeshi Masumoto | Manufacture of flaky rapidly cooling solidified metal powder |
| US5993509A (en) * | 1996-11-19 | 1999-11-30 | Nat Science Council | Atomizing apparatus and process |
| CN1257767A (en) * | 1998-12-23 | 2000-06-28 | 江苏江南铁合金厂 | Process for preparing tin particles |
| CN101202170A (en) * | 2007-10-23 | 2008-06-18 | 福达合金材料股份有限公司 | Method of preparing sheet silver tin oxide electrical contact material |
| JP2009249702A (en) * | 2008-04-08 | 2009-10-29 | Hitachi Metals Ltd | Magnetic alloy powder, and method for producing the same |
| CN203791631U (en) * | 2013-12-27 | 2014-08-27 | 重庆华浩冶炼有限公司 | Tin powder atomizing barrel |
-
2014
- 2014-05-22 CN CN201410216580.8A patent/CN103934462A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH024906A (en) * | 1988-06-22 | 1990-01-09 | Takeshi Masumoto | Manufacture of flaky rapidly cooling solidified metal powder |
| US5993509A (en) * | 1996-11-19 | 1999-11-30 | Nat Science Council | Atomizing apparatus and process |
| CN1257767A (en) * | 1998-12-23 | 2000-06-28 | 江苏江南铁合金厂 | Process for preparing tin particles |
| CN101202170A (en) * | 2007-10-23 | 2008-06-18 | 福达合金材料股份有限公司 | Method of preparing sheet silver tin oxide electrical contact material |
| JP2009249702A (en) * | 2008-04-08 | 2009-10-29 | Hitachi Metals Ltd | Magnetic alloy powder, and method for producing the same |
| CN203791631U (en) * | 2013-12-27 | 2014-08-27 | 重庆华浩冶炼有限公司 | Tin powder atomizing barrel |
Non-Patent Citations (2)
| Title |
|---|
| 刘维平 等: "锡深加工及锡粉制备", 《矿冶工程》, vol. 25, no. 6, 31 December 2005 (2005-12-31), pages 66 - 69 * |
| 陈文汩 等: "气体雾化法制备锡粉的技术研究", 《粉末冶金工业》, vol. 12, no. 3, 30 June 2002 (2002-06-30), pages 33 - 69 * |
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Application publication date: 20140723 |