CN105731529A - Method for preparing tin tetrachloride by jet process - Google Patents
Method for preparing tin tetrachloride by jet process Download PDFInfo
- Publication number
- CN105731529A CN105731529A CN201610053680.2A CN201610053680A CN105731529A CN 105731529 A CN105731529 A CN 105731529A CN 201610053680 A CN201610053680 A CN 201610053680A CN 105731529 A CN105731529 A CN 105731529A
- Authority
- CN
- China
- Prior art keywords
- tin
- aerochamber
- chlorine
- roller
- fluid
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- 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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Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/04—Halides
- C01G19/08—Stannic chloride
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention relates to the field of deep processing of tin and particularly relates to a method for preparing tin tetrachloride by a jet process. The method comprises the following steps: melting tin particles; jetting the molten fluid vertically from top to bottom to the surface of a roller in high-speed rotation through a nozzle, wherein the fluid is thrown to an atomizing chamber on one side through the roller rotation and forms tin drops; introducing chlorine gas into the atomizing chamber from bottom to top so that the chlorine gas reacts with the tin drops; discharging the chlorine gas remaining after the reaction from the upper side of the atomizing chamber and collecting; enabling the liquid-state tin tetrachloride generated by the reaction to flow out from the lower side of the atomizing chamber, and collecting; and conveying the collected chlorine gas to the atomizing chamber again for recycling. In the invention, the jet fluid is broken by the centrifugal force of the rotating roller, and the tin drops are hit by the high-speed chlorine gas so that the the jet fluid and the tin drops are sufficiently mixed for reaction; under the effect of gravity, the generated tin tetrachloride always flows to the bottom of the atomizing chamber from top to bottom, thus the reaction is sufficient, and the product quality can be improved; and moreover, continuous production can be carried out, and the yield can be increased.
Description
Technical field
The present invention relates to the field of deep of stannum, the method that specifically spurt method prepares butter of tin.
Background technology
Butter of tin is the primary raw material of organo-tin compound, and the organo-tin compound world for PVC product with as heat stabilizer consumes consumption to be increased year by year.Anhydrous stannic chloride can be used as raw material and the chlorinating agent of organotin synthesis, soft dose of the coal in textile industry, manufactures blueprint paper, sensitive paper, lubrication oil additive and the field such as tin plating.At present, the contract of most of butters of tin is all with the intermittent operation of metallic tin grain or anhydrous stannous chloride and chlorine reaction.When preparation amount is bigger, it is necessary to the stopped reaction of midway, one after another liquid product is taken out, then supplement stannum grain, be further continued for passing into chlorine.This method complex operation, is fiercely fuming during transfer product, and degradation manipulation environment, combined coefficient and quality are affected.And the gas-solid reaction mode of this metallic tin grain and chlorine needs to consume substantial amounts of metallic tin, and reaction yield is low, and productivity is relatively low.
Summary of the invention
For the problems referred to above, the present invention provides a kind of productivity higher and can the quantity-produced spurt method method of preparing butter of tin.
This invention address that the technical scheme that above-mentioned technical problem adopts is: spurt method prepares the method for butter of tin, comprises the following steps:
(1) molten tin grain；
(2) fluid after melted is vertically sprayed the roller surface to high speed rotating from top to bottom by nozzle；
(3) fluid rotates the aerochamber got rid of to side through roller, forms stannum and drips；
(4) in aerochamber, pass into chlorine from bottom to top drip reaction with stannum；
(5) react remaining chlorine to be discharged by the upside of aerochamber, and collect；
(6) the liquid butter of tin that reaction generates flows out on the downside of aerochamber, and collects；
(7) chlorine collected again is delivered to aerochamber and recycles.
As preferably, described roller surface offers several spherical groove；Injection flows to groove to the fluid of roller surface, and the fluid in groove gets rid of to aerochamber.
As preferably, groove is 0.5 1mm at the opening diameter of roller surface.
As preferably, the mass flowrate of fluid jet is 6 8g/s.
As preferably, the vertical dimension between nozzle and roller is 0.01 0.1mm, and the diameter of roller is 40 50mm, and roller rotating speed is 300-350r/min.
As preferably, in aerochamber, the flow direction of chlorine and the angle of horizontal direction are 45 °--90 °.
As preferably, the flow velocity of chlorine is 30m/s, and the flow of chlorine is 0.1 0.15m3/h。
As preferably, keeping reaction temperature in aerochamber is 100 145 DEG C.
As preferably, the chlorine of collection is delivered to aerochamber by air pump.
The fluid of injection is smashed by the present invention by the centrifugal force of swing roller, clash into stannum again through high speed chlorine to drip so that both are sufficiently mixed reaction, and the butter of tin of generation can be made under gravity to flow to from top to bottom all the time bottom aerochamber, not only reaction fully, can improve the quality of product；And can produce continuously, productivity can be improved.
Detailed description of the invention
The present invention is described more detail below, and illustrative examples and explanation in this present invention are used for explaining the present invention, but not as a limitation of the invention.
The spurt method of the present invention prepares the method for butter of tin, and it adopts following steps:
First stannum grain is melted, more melted stannum fluid is vertically sprayed the roller surface to high speed rotating by nozzle；Roller surface offers several spherical groove, and the fluid that can spray to roller surface flows to groove, extends the fluid time of staying on surface so that it is suitably cool down, so make the fluid in groove get rid of to the epigranular degree after aerochamber better；In order to avoid fluid time of staying on surface is long, cause that powder diameter is excessive, the groove of the present invention is advisable with 0.5 1mm at the opening diameter of roller surface, and should ensure that the mass flowrate of fluid jet be the vertical dimension between 6 8g/s, nozzle and roller is 0.01 0.1mm, the roller diameter simultaneously adopted is 40 50mm, and roller rotating speed is 300-350r/min；Getting rid of the stannum to aerochamber to drip and clashed into by high speed chlorine, stannum can be made to drip on the one hand broken, both flow directions can be sufficiently mixed reaction on the contrary on the other hand；In aerochamber, the flow direction of chlorine and the angle of horizontal direction are preferably 45 °--90 °, such crushing effect is better；In implementation process, the flow velocity of chlorine keeps 30m/s to be advisable, and flow is with 0.1 0.15m3/ h is advisable；Should ensure that the reaction temperature in aerochamber is at 100 145 DEG C simultaneously, drip for stannum and fully react the condition providing good with chlorine.From the chlorine of aerochamber upper collection, first it is storable in air accumulator, the aerochamber then again chlorine in air accumulator carried by high-pressure pump, so recycles chlorine, not only can reduce the cost recovery of chlorine, and the requirement that cleaning produces can be reached；After completion of the reaction, stop passing into chlorine, chlorine can be collected on the upside of aerochamber, it is to avoid cause environmental pollution；And the butter of tin generated flows to bottom aerochamber under gravity, so collect more convenient, it is not necessary to midway is suspended.
Embodiment 1
Stannum grain is melted, then molten tin fluid is vertically sprayed to the reeded roller surface of tool rotated by nozzle；Its further groove is 0.5mm, mass flowrate to be the vertical dimension between 6g/s, nozzle and roller the be 0.01mm of fluid jet, roller diameter at the opening diameter of roller surface is 40mm, and roller rotating speed is 300r/min；Meanwhile, in aerochamber, to keep 45 ° of angles with horizontal direction, and with 0.15m3/ h, 30m/s flow velocity pass into chlorine clash into stannum drip and react, reaction temperature maintains 100 DEG C, finally from aerochamber bottom collection butter of tin.By analysis, the purity of butter of tin about 99.2%, whole building-up process productivity reaches 85%.
Embodiment 2
Stannum grain is melted, then molten tin fluid is vertically sprayed to the reeded roller surface of tool rotated by nozzle；Its further groove is 0.7mm, mass flowrate to be the vertical dimension between 7g/s, nozzle and roller the be 0.05mm of fluid jet, roller diameter at the opening diameter of roller surface is 45mm, and roller rotating speed is 320r/min；Meanwhile, in aerochamber, to keep 60 ° of angles and with 0.12m with horizontal direction3/ h, 30m/s flow velocity pass into chlorine clash into stannum drip and react, reaction temperature maintains 125 DEG C, finally from aerochamber bottom collection butter of tin.By analysis, the purity of butter of tin about 99.8%, whole building-up process productivity reaches 89%.
Embodiment 3
Stannum grain is melted, then molten tin fluid is vertically sprayed to the reeded roller surface of tool rotated by nozzle；Its further groove is 1.0mm, mass flowrate to be the vertical dimension between 8g/s, nozzle and roller the be 0.1mm of fluid jet, roller diameter at the opening diameter of roller surface is 42mm, and roller rotating speed is 350r/min；Meanwhile, in aerochamber, to keep 90 ° of angles with horizontal direction, and with 0.1m3/ h, 30m/s flow velocity pass into chlorine clash into stannum drip and react, reaction temperature maintains 145 DEG C, finally from aerochamber bottom collection butter of tin.By analysis, the purity of butter of tin about 99.5%, whole building-up process productivity reaches 83%.
The technical scheme above embodiment of the present invention provided is described in detail, principle and the embodiment of the embodiment of the present invention are set forth by specific case used herein, and the explanation of above example is only applicable to help to understand the principle of the embodiment of the present invention；Simultaneously for one of ordinary skill in the art, according to the embodiment of the present invention, all will change in detailed description of the invention and range of application, in sum, this specification content should not be construed as limitation of the present invention.
Claims (9)
1. the method that spurt method prepares butter of tin, comprises the following steps:
(1) molten tin grain；
(2) fluid after melted is vertically sprayed the roller surface to high speed rotating from top to bottom by nozzle；
(3) fluid rotates the aerochamber got rid of to side through roller, forms stannum and drips；
(4) in aerochamber, pass into chlorine from bottom to top drip reaction with stannum；
(5) react remaining chlorine to be discharged by the upside of aerochamber, and collect；
(6) the liquid butter of tin that reaction generates flows out on the downside of aerochamber, and collects；
(7) chlorine collected again is delivered to aerochamber and recycles.
2. the method that spurt method prepares butter of tin according to claim 1, it is characterised in that: described roller surface offers several spherical groove；Injection flows to groove to the fluid of roller surface, and the fluid in groove gets rid of to aerochamber.
3. the method that spurt method prepares butter of tin according to claim 2, it is characterised in that: groove is 0.5 1mm at the opening diameter of roller surface.
4. the method that spurt method prepares butter of tin according to claim 3, it is characterised in that: the mass flowrate of fluid jet is 6 8g/s.
5. the method that spurt method according to any one in Claims 1-4 prepares butter of tin, it is characterised in that: the vertical dimension between nozzle and roller is 0.01 0.1mm, and the diameter of roller is 40 50mm, and roller rotating speed is 300-350r/min.
6. the method that spurt method prepares butter of tin according to claim 5, it is characterised in that: in aerochamber, the flow direction of chlorine and the angle of horizontal direction are 45 °--90 °.
7. the method that spurt method prepares butter of tin according to claim 6, it is characterised in that: the flow velocity of chlorine is 30m/s, and the flow of chlorine is 0.1 0.15m3/h。
8. the method that spurt method prepares butter of tin according to claim 7, it is characterised in that: keeping reaction temperature in aerochamber is 100 145 DEG C.
9. the method that spurt method prepares butter of tin according to claim 1, it is characterised in that: the chlorine of collection is delivered to aerochamber by air pump.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610053680.2A CN105731529A (en) | 2016-01-27 | 2016-01-27 | Method for preparing tin tetrachloride by jet process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610053680.2A CN105731529A (en) | 2016-01-27 | 2016-01-27 | Method for preparing tin tetrachloride by jet process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105731529A true CN105731529A (en) | 2016-07-06 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610053680.2A Pending CN105731529A (en) | 2016-01-27 | 2016-01-27 | Method for preparing tin tetrachloride by jet process |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006213986A (en) * | 2005-02-07 | 2006-08-17 | Minerva Kiki Kk | Method for producing fine metallic powder and production apparatus therefor |
| CN102180514A (en) * | 2011-03-05 | 2011-09-14 | 招远市松鹤化工有限公司 | Production process of tin tetrachloride |
-
2016
- 2016-01-27 CN CN201610053680.2A patent/CN105731529A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006213986A (en) * | 2005-02-07 | 2006-08-17 | Minerva Kiki Kk | Method for producing fine metallic powder and production apparatus therefor |
| CN102180514A (en) * | 2011-03-05 | 2011-09-14 | 招远市松鹤化工有限公司 | Production process of tin tetrachloride |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
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| RJ01 | Rejection of invention patent application after publication | ||
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Application publication date: 20160706 |