CN105731528A - Preparation method of stannic chloride - Google Patents
Preparation method of stannic chloride Download PDFInfo
- Publication number
- CN105731528A CN105731528A CN201610053678.5A CN201610053678A CN105731528A CN 105731528 A CN105731528 A CN 105731528A CN 201610053678 A CN201610053678 A CN 201610053678A CN 105731528 A CN105731528 A CN 105731528A
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- CN
- China
- Prior art keywords
- chlorine
- aerochamber
- tin
- butter
- preparation
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Classifications
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- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Dairy Products (AREA)
Abstract
The invention relates to the further processing field of tin, and in particular relates to a preparation method of stannic chloride. The preparation method comprises the following steps: melting tin particles; vertically injecting molten fluid from top to bottom to the surface of a roller rotating at a high speed by virtue of a spray nozzle; spinning the fluid to an atomizing chamber at one side by virtue of the roller to form tin drops; introducing chlorine into the atomizing chamber from bottom to top to react with the tin drops; injecting a mixture to a collection chamber at one side of the atomizing chamber; collecting the chlorine at the upper side of the collection chamber; collecting liquid stannic chloride at the lower side of the collection chamber; and re-conveying the collected chlorine to the atomizing chamber to be recycled. The injected fluid is crushed by virtue of the centrifugal force of the rotating roller, and the tin drops collide with the high-speed chlorine, so that the chlorine is sufficiently mixed with the tin drops, and reactants are sufficiently mixed; and then the reactants are injected to the collection chamber by virtue of an injector, so that the collection of products and the chlorine is greatly facilitated.
Description
Technical field
The present invention relates to the field of deep of stannum, specifically butter of tin preparation method.
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 quantity-produced butter of tin preparation method.
This invention address that the technical scheme that above-mentioned technical problem adopts is: butter of tin preparation method, comprise 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) again by the collecting chamber of mixture injection to aerochamber side;
(6) on the upside of collecting chamber, collect chlorine, on the downside of collecting chamber, collect liquid butter of tin;
(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, being provided with ejector in aerochamber, the mixture in aerochamber is by ejector injection to collecting chamber.
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, clashes into stannum again through high speed chlorine and drips so that both are sufficiently mixed reaction, and reactant can be made to be sufficiently mixed, then passes through ejector and spray to collecting chamber, significantly facilitate the collection of product and chlorine;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 preparation method of the butter of tin of the present invention, 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;After reaction, mixture is sprayed to collecting chamber again by ejector, the mixture not having complete reaction so can be made to form certain pressure by ejector so that it is complete reaction, improves productivity;Having pressure owing to passing into the chlorine itself in aerochamber, only at the side-wall hole of aerochamber, then need to install ejector in hole and achieve that injection, therefore, processing is simple, and cost is low;Spraying into the mixture in collecting chamber is butter of tin and chlorine, and both are different due to density, can separate under gravity, therefore can collect chlorine on the upside of collecting chamber, and product is collected in downside, so collects more convenient, it is not necessary to midway is suspended.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;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.
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;Then the mixture in aerochamber sprays to collecting chamber, finally from collecting chamber bottom collection butter of tin.By analysis, the purity of butter of tin about 99.3%, whole building-up process productivity reaches 88%.
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, then the mixture in aerochamber spray to collecting chamber, finally from collecting chamber bottom collection butter of tin.By analysis, the purity of butter of tin about 99.9%, whole building-up process productivity reaches 93%.
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, then the mixture in aerochamber spray to collecting chamber, finally from collecting chamber bottom collection butter of tin.By analysis, the purity of butter of tin about 99.4%, whole building-up process productivity reaches 90%.
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 (10)
1. the preparation method of 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) again by the collecting chamber of mixture injection to aerochamber side;
(6) on the upside of collecting chamber, collect chlorine, on the downside of collecting chamber, collect liquid butter of tin;
(7) chlorine collected again is delivered to aerochamber and recycles.
2. the preparation method of 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 preparation method of 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 preparation method of butter of tin according to claim 3, it is characterised in that: the mass flowrate of fluid jet is 6 8g/s.
5. the preparation method of butter of tin according to any one in Claims 1-4, 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 preparation method of 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 preparation method of 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 preparation method of butter of tin according to claim 7, it is characterised in that: keeping reaction temperature in aerochamber is 100 145 DEG C.
9. the preparation method of butter of tin according to claim 1, it is characterised in that: being provided with ejector in aerochamber, the mixture in aerochamber is by ejector injection to collecting chamber.
10. the preparation method of 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)
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CN201610053678.5A CN105731528A (en) | 2016-01-27 | 2016-01-27 | Preparation method of stannic chloride |
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CN201610053678.5A CN105731528A (en) | 2016-01-27 | 2016-01-27 | Preparation method of stannic chloride |
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CN201610053678.5A Pending CN105731528A (en) | 2016-01-27 | 2016-01-27 | Preparation method of stannic chloride |
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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 CN201610053678.5A patent/CN105731528A/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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Application publication date: 20160706 |