CN105731530A - Tin tetrachloride production device with wave tube reactor - Google Patents
Tin tetrachloride production device with wave tube reactor Download PDFInfo
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- CN105731530A CN105731530A CN201610274775.7A CN201610274775A CN105731530A CN 105731530 A CN105731530 A CN 105731530A CN 201610274775 A CN201610274775 A CN 201610274775A CN 105731530 A CN105731530 A CN 105731530A
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- tin
- wave duct
- melting furnace
- tube
- duct reactor
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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
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- 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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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention discloses a tin tetrachloride production device with a wave tube reactor. The tin tetrachloride production device comprises a tin smelting furnace, a pressurizing tank, a condensing tube, a chlorine gas storage tank, a cyclone separating tank and a product storage tank, wherein the tin smelting furnace is connected to the pressurizing tank; the interior of the tin smelting furnace is provided with the wave tube reactor; the wave tube reactor comprises a reaction pipeline with a tube body as a wave tube body, two inlet tubes and a product outlet tube; the bottom of the pressurizing tank is connected with a tin liquor feeding tube; the tail end of the tin liquor feeding tube is connected to any inlet tube of the wave tube reactor; the outlet of the chlorine gas storage tank is connected with a tee joint; one outlet of the tee joint is connected to the other inlet tube of the wave tube reactor through the chlorine gas inlet tube; another outlet of the tee joint is connected to the top of the cyclone separating tank; the product outlet tube of the wave tube reactor is connected to the cyclone separating tank through the condensing tube; the bottom of the cyclone separating tank is connected to the product storage tank. The tin tetrachloride production device not only can realize continuous production, but also can be high in reaction speed, high in yield and almost free of pollution on environment.
Description
Technical field
The invention belongs to chemical production equipment field, be specifically related to a kind of butter of tin process units with wave duct reactor.
Background technology
Current chemical reaction equipment substantially can be divided three classes: 1. reactor (tank, groove)；2. reaction (absorption) tower；3. reaction tube.1., 2. not only cost is high, but also there is the problem that heating is uneven or heat release is not easily discharged, and this is also one of Chemical Manufacture main contributor being usually present enlarge-effect；Additionally, chemical reaction generally requires stirring, this just faces sealing problem, especially for high pressure, pyroreaction and need the reaction of high-speed stirred, will solve sealing problem just increasingly difficult, even can not solve.Although disadvantages mentioned above 1., 2. 3. can be overcome, but himself there is no the ability of good mixed reactant, so that another reactant ligand thing mixing stirring device.Certainly, also there is the fixing blade that different distributions direction is set in reaction tube to realize the pipe reaction device that reactant not only mixes but also reacts, but such device is again because resistance is more greatly, usually block, thus range of application is limited.It is true that from bionic angle, what reactor, reaction tower and the tubular reactor with blocking vane, be simply all non-existent in vivo." stomach " of animal although similar reactor, but it is except having preliminary digestive function, more importantly memory function, and has " organ " of Wave-shaped structural, such as " intestinal ", " blood vessel ", " lymphoid tissue " etc., then all there is the function of " chemical reactor ".Plant also has homologous organs, and this ought to give people with enlightenment.
Butter of tin is the basic raw material of organo-tin compound.Its synthesis has " Xi Si-chlorine " under low temperature (150 DEG C) condition and " tin liquor-chlorine " the two kinds of reaction process under high temperature (250～300 DEG C) condition.
The course of reaction of stannum and chlorine is
First step Sn+Cl2→SnCl2(fusing point 246 DEG C, boiling point 652 DEG C)
Second step SnCl2+Cl2→SnCl4(fusing point-33 DEG C, boiling point 114.1 DEG C)
The fusing point of known metal stannum is fusing point 231.88 DEG C, boiling point 2270 DEG C, therefore during low-temp reaction, although the temperature on stannum silk surface can exceed that the fusing point of metallic tin, but stannum silk outermost layer necessarily drapes over one's shoulders multiple one layer of stannous chloride solid or liquid, therefore second step reaction must be the most rapid of decision overall reaction rate.Therefore, low-temp reaction existing problems are that response speed is slow, and can only batch production, the impurity content that its advantage is thick product is low, but the requirement reaching GB 622-89 is still not fee from redistillation；Although pyroreaction can produce continuously, but owing to tin liquor is relatively big with the density contrast of chlorine, the speed of chlorine bubbles effusion tin liquor is fast, and this necessarily affects response speed.Furthermore, supplementary block tin easily causes again the pollution to environment of chlorine and butter of tin.
Summary of the invention
For solving above-mentioned technical problem, the present invention provides a kind of butter of tin process units with wave duct reactor, and this device is possible not only to realize continuous production, and response speed is fast, and productivity is high, to environment almost without pollution.
The technical solution adopted in the present invention is: have the butter of tin process units of wave duct reactor, including tin melting furnace, pressurized canister, condensing tube, chlorine storage tank, cyclonic separation tank and product storage tank, the top of described tin melting furnace offers charge door, the bottom of tin melting furnace is connected with pressurized canister by tin liquor charger, the inside of tin melting furnace is provided with wave duct reactor, and wave duct reactor includes reacting pipe that body is waveform body, is arranged on two inlet tubes of reacting pipe one end, is arranged on the product outlet tube of the reacting pipe other end；The bottom of described pressurized canister is connected to tin liquor feed pipe, and the end of tin liquor feed pipe is connected to one of them inlet tube of wave duct reactor；The outlet of described chlorine storage tank is connected to threeway, and one of them outlet of threeway is connected to the another one inlet tube of wave duct reactor by chlorine air inlet pipe, and another outlet of threeway is connected to cyclonic separation tank top；The product outlet tube of described wave duct reactor is connected to cyclonic separation tank by condensing tube, and the bottom of cyclonic separation tank is connected to product storage tank.
Have the further optimization of the butter of tin process units of wave duct reactor as the present invention, the internal diameter of the reacting pipe of described wave duct reactor tapers into along material conveying direction.
There is the further optimization of the butter of tin process units of wave duct reactor as the present invention, the reacting pipe of described wave duct reactor is the waveform pipeline that multiple curved pipe is sequentially connected with composition, and the wave amplitude of waveform pipeline and/or wavelength are gradually reduced along material conveying direction.
There is the further optimization of the butter of tin process units of wave duct reactor as the present invention, the cooling tube of U-shape structure it is additionally provided with in described tin melting furnace, the entrance point of cooling tube stretch out tin melting furnace and by threeway respectively with blower fan and cool down water storage tank, the port of export of cooling tube stretches out tin melting furnace and atmosphere.
Have the further optimization of the butter of tin process units of wave duct reactor as the present invention, the top of described pressurized canister is connected to nitrogen storage tank, is provided with relief valve between pressurized canister and nitrogen storage tank.
There is as the present invention the further optimization of the butter of tin process units of wave duct reactor, in described tin melting furnace, pressurized canister and cyclonic separation tank, be equipped with temperature probe.
There is as the present invention the further optimization of the butter of tin process units of wave duct reactor, the sidewall of described tin melting furnace and pressurized canister is equipped with form.
Have the further optimization of the butter of tin process units of wave duct reactor as the present invention, the bottom of described tin melting furnace is provided with atmospheric valve I, and the side of tin melting furnace is provided with scruff discharge nozzle.
Have the further optimization of the butter of tin process units of wave duct reactor as the present invention, described tin liquor feed pipe is provided with overrun control.
Having the further optimization of the butter of tin process units of wave duct reactor as the present invention, be provided with drain pipe bottom described pressurized canister, drain pipe connects tin liquor feed pipe by threeway one end, and the other end is connected to atmospheric valve II.
Compared with prior art, the present invention at least has and has the advantage that and beneficial effect:
The butter of tin process units with wave duct reactor provided by the invention is possible not only to realize continuous production, and response speed is fast, and productivity is high, to environment almost without pollution.In the present invention, the hybrid reaction of tin liquor and chlorine carries out in the wave duct reactor that body is waveform body, reaction contact area not only can be made to increase and continual and steady, thus improving response speed, and whole response system is in sealing state, make environmental pollution greatly reduce, fully achieve the requirement of GB 622-89 through overweight steaming product.
Accompanying drawing explanation
Fig. 1 is the structural representation of the present invention；
Accompanying drawing labelling: 1, tin melting furnace, 2, pressurized canister, 3, condensing tube, 4, cyclonic separation tank, 5, product storage tank, 6, charge door, 7, tin liquor charger, 8, reacting pipe, 9, inlet tube, 10, outlet, 11, relief valve, 12, tin liquor feed pipe, 13, chlorine air inlet pipe, 14, cooling tube, 15, blower fan, 16, cooling water storage tank, 17, temperature probe, 18, form, 19, atmospheric valve I, 20, scruff discharge nozzle, 21, overrun control, 22, drain pipe, 23, atmospheric valve II.
Detailed description of the invention
For making present disclosure become apparent, below in conjunction with specific embodiment, describe the present invention.
As shown in the figure, there is the butter of tin process units of wave duct reactor, including tin melting furnace 1, pressurized canister 2, condensing tube 3, chlorine storage tank, cyclonic separation tank 4 and product storage tank 5, the top of described tin melting furnace 1 offers charge door 6, the bottom of tin melting furnace 1 is connected with pressurized canister 2 by tin liquor charger 7, the inside of tin melting furnace 1 is provided with wave duct reactor, and wave duct reactor includes reacting pipe 8 that body is waveform body, is arranged on two inlet tubes 9 of reacting pipe 8 one end, is arranged on the product outlet tube 10 of reacting pipe 8 other end；The bottom of described pressurized canister 2 is connected to tin liquor feed pipe 12, and the end of tin liquor feed pipe 12 is connected to one of them inlet tube 9 of wave duct reactor；The outlet of described chlorine storage tank is connected to threeway, and one of them outlet of threeway is connected to the another one inlet tube 9 of wave duct reactor by chlorine air inlet pipe 13, and another outlet of threeway is connected to cyclonic separation tank 4 top；The product outlet tube 10 of described wave duct reactor is connected to cyclonic separation tank 4 by condensing tube 3, and the bottom of cyclonic separation tank 4 is connected to product storage tank 5.
In order to make the present invention have better implementation result, the internal diameter of the reacting pipe 8 of described wave duct reactor tapers into along material conveying direction, the reacting pipe 8 of wave duct reactor is the waveform pipeline that multiple curved pipe is sequentially connected with composition, and the wave amplitude of waveform pipeline and/or wavelength are gradually reduced along material conveying direction.Described wave amplitude refers to the height of each curved pipe vibration in waveform reaction tube, and wavelength is the width of each curved pipe.Wherein curved pipe and curved pipe all connect mode with kiss and are end-to-end, and two arcs that connect lay respectively at their both sides (the following stated " kiss of arc and arc connects " refers both to this kind of mode) of common tangent, and two ends straight pipeline and curved pipe also connect mode be connected to kiss.
In the present invention, in described tin melting furnace 1, be additionally provided with the cooling tube 14 of U-shape structure, the entrance point of cooling tube 14 stretch out tin melting furnace 1 and by threeway respectively with blower fan 15 and cool down water storage tank 16, the port of export of cooling tube 14 stretches out tin melting furnace 1 and atmosphere.
As preferrred embodiment of the present invention, the top of described pressurized canister 2 is connected to nitrogen storage tank, is provided with relief valve 11 between pressurized canister 2 and nitrogen storage tank.It is equipped with temperature probe 17 in described tin melting furnace 1, pressurized canister 2 and cyclonic separation tank 4.The sidewall of described tin melting furnace 1 and pressurized canister 2 is equipped with form 18.The bottom of described tin melting furnace 1 is provided with atmospheric valve I 19, and the side of tin melting furnace 1 is provided with scruff discharge nozzle 20.Described tin liquor feed pipe 12 is provided with overrun control 21.Being provided with drain pipe 22 bottom described pressurized canister 2, drain pipe 22 connects tin liquor feed pipe 12 by threeway one end, and the other end is connected to atmospheric valve II 23.Being provided with a baffle plate near the position of outlet in cyclonic separation tank 4, three legs of baffle plate are uniform.
The process units of the present invention is as shown in the figure, in figure, the material of wave duct reactor is quartz glass tube, and tin melting furnace 1, pressurized canister 2 are conventional refractory materials equipment, the preferred quartz glass of material of tin liquor charger 7, can also be graphite or fluoroplastics, the shell of condensing tube 3 and the material of cooling tube 14 are rustless steel, and the blower fan being placed in cyclonic separation tank 4 top is fluoroplastics centrifugal pump, and blower fan 15 is carbon steel material, cyclonic separation tank 4 is fluoroplastics, and the pipe fitting of identical material joined by the pipe of relevant materials.
The concrete operation method of the present invention is as follows:
1, measuring and controlling equipment is opened, including the temperature probe 17 being equipped with in tin melting furnace 1, pressurized canister 2 and cyclonic separation tank 4, the power supply of pressure transducer 39, open atmospheric valve 26, nitrogen is passed into pressurized canister 2 with nitrogen pot, close atmospheric valve II 23 after getting rid of air therein, open the product baiting valve bottom cyclonic separation tank 4, the switch valve on tin liquor feed pipe 12 and the electromagnetic valve on overrun control 21, discharge the air in product outlet tube 10 and cyclonic separation tank 4；Open and be placed in the choke valve in the blower fan at cyclonic separation tank 4 top, chlorine air inlet pipe 13, the switch valve between chlorine storage tank and cyclonic separation tank 4 top, continue logical nitrogen after more than 10 minutes, close the product baiting valve bottom cyclonic separation tank 4 and be placed in the blower fan at cyclonic separation tank 4 top.
2, temperature control 250 DEG C is set, it is energized to the heater strip of tin melting furnace 1, open tin liquor charger 7, nitrogen enters tin melting furnace by tin liquor charger 7, and 1, by charge door 6, and when avoiding percussion wave pipe reactor, in tin melting furnace 1, add stannum grain carefully, observed by form 18, make the upper interface that stannum grain is piled be positioned at the middle and upper part of form 18.
3, when temperature is more than more than 232 DEG C, stannum grain melts and flows into tin liquor charger 7, and along with the operating of tin liquor charger 7, tin liquor enters pressurized canister 2, and nitrogen enters tin melting furnace 1.
4, after the liquid level in pressurized canister 2 enters the middle and lower part of form 18, open the cooling water of condensing tube 3, pass into dry chlorine gas, and open the blower fan being placed in cyclonic separation tank 4 top, regulate the choke valve in chlorine air inlet pipe 13, the reading making the effusion meter in chlorine air inlet pipe 13 is 300L/min, the pressure the open time delay that increase nitrogen control device 21, and the flow making tin liquor is 0.69kg/min.
5, according to the temperature controller probe measured temperature on cyclonic separation tank, by " chlorine flowrate-temperature " curve, choke valve or overrun control are regulated in real time, it is ensured that stannum and chlorine react by the mol ratio of 1: 2.
6, along with the carrying out of reaction, the heater strip of tin melting furnace 1 is automatically stopped heating under the control of temperature controller, when displays temperature is still above 300 DEG C, blower fan 15 should be opened, if temperature continues to raise the distillation water control valve that also should suitably open cooling water storage tank 16 place, the evaporation latent heat of a small amount of distilled water and the thermal conductivity ratio air of steam is utilized to reduce the temperature of tin melting furnace 1 greatly further.
If the scruff accumulation in 7 tin melting furnaces 1 is more, the scruff outlet valve that should open scruff discharge nozzle 20 place is discharged in time.
8, observing the liquid level of liquidometer on cyclonic separation tank 4, the butter of tin released containing a small amount of chlorine goes out product in time, is further purified technique.
When 9, temporarily ceasing reaction, first nitrogen supply (NS) should be cut off and open relief valve 11, allow the molten tin backflow in part pipe to pressurized canister 2, close overrun control 21, cut off chlorine source of supply, connect nitrogen cylinder, after allowing the chlorine of residual continue reaction with tin liquor, stop blower fan and cooling water, stop blower fan II 55 and close distillation water control valve 56.
10, maintenance is monthly stopped production once, during stopping production, also on the basis of the 9th step, relief valve 11 should be closed and continue to pass into nitrogen, opening atmospheric valve II 23, release the tin liquor in tin melting furnace 1 and pressurized canister 2, it is down to after room temperature until temperature, unloads wave duct reactor and cooling tube 14, and the solid adhesion processed on wave duct reactor wall with dust technology is mainly lead chloride, copper chloride and bismuth chloride, then clean with distilled water flushing, install again after drying, use.
Adopting assembly of the invention, every year by 200 days, continuous 24 small-scale productions calculating, can produce the thick product 200 tons more than containing butter of tin 95% mass, wherein major impurity is excess chlorine.Add stannum grain or stannum silk heavily steams, collect through inspection the present embodiment product every physical and chemical index such as following table.
。
Claims (10)
1. there is the butter of tin process units of wave duct reactor, it is characterized in that: include tin melting furnace (1), pressurized canister (2), condensing tube (3), chlorine storage tank, cyclonic separation tank (4) and product storage tank (5), the top of described tin melting furnace (1) offers charge door (6), the bottom of tin melting furnace (1) is connected with pressurized canister (2) by tin liquor charger (7), the inside of tin melting furnace (1) is provided with wave duct reactor, wave duct reactor includes the reacting pipe (8) that body is waveform body, it is arranged on two inlet tubes (9) of reacting pipe (8) one end, it is arranged on the product outlet tube (10) of reacting pipe (8) other end；The bottom of described pressurized canister (2) is connected to tin liquor feed pipe (12), and the end of tin liquor feed pipe (12) is connected to one of them inlet tube (9) of wave duct reactor；The outlet of described chlorine storage tank is connected to threeway, and one of them outlet of threeway is connected to the another one inlet tube (9) of wave duct reactor by chlorine air inlet pipe (13), and another outlet of threeway is connected to cyclonic separation tank (4) top；The product outlet tube (10) of described wave duct reactor is connected to cyclonic separation tank (4) by condensing tube (3), and the bottom of cyclonic separation tank (4) is connected to product storage tank (5).
2. there is the butter of tin process units of wave duct reactor as claimed in claim 1, it is characterised in that: the internal diameter of the reacting pipe (8) of described wave duct reactor tapers into along material conveying direction.
3. there is the butter of tin process units of wave duct reactor as claimed in claim 1 or 2, it is characterized in that: the reacting pipe (8) of described wave duct reactor is sequentially connected with the waveform pipeline of composition for multiple curved pipes, and the wave amplitude of waveform pipeline and/or wavelength are gradually reduced along material conveying direction.
4. there is the butter of tin process units of wave duct reactor as claimed in claim 1, it is characterized in that: in described tin melting furnace (1), be additionally provided with the cooling tube (14) of U-shape structure, the entrance point of cooling tube (14) stretch out tin melting furnace (1) and by threeway respectively with blower fan (15) and cool down water storage tank (16), the port of export of cooling tube (14) stretches out tin melting furnace (1) and atmosphere.
5. there is the butter of tin process units of wave duct reactor as claimed in claim 1, it is characterised in that: the top of described pressurized canister (2) is connected to nitrogen storage tank, is provided with relief valve (11) between pressurized canister (2) and nitrogen storage tank.
6. there is the butter of tin process units of wave duct reactor as claimed in claim 1, it is characterised in that: it is equipped with temperature probe (17) in described tin melting furnace (1), pressurized canister (2) and cyclonic separation tank (4).
7. there is the butter of tin process units of wave duct reactor as claimed in claim 1, it is characterised in that: the sidewall of described tin melting furnace (1) and pressurized canister (2) is equipped with form (18).
8. there is the butter of tin process units of wave duct reactor as claimed in claim 1, it is characterised in that: the bottom of described tin melting furnace (1) is provided with atmospheric valve I (19), and the side of tin melting furnace (1) is provided with scruff discharge nozzle (20).
9. there is the butter of tin process units of wave duct reactor as claimed in claim 1, it is characterised in that: described tin liquor feed pipe (12) is provided with overrun control (21).
10. there is the butter of tin process units of wave duct reactor as claimed in claim 1, it is characterized in that: described pressurized canister (2) bottom is provided with drain pipe (22), drain pipe (22) connects tin liquor feed pipe (12) by threeway one end, and the other end is connected to atmospheric valve II (23).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610274775.7A CN105731530B (en) | 2016-04-28 | 2016-04-28 | Butter of tin process units with wave duct reactor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610274775.7A CN105731530B (en) | 2016-04-28 | 2016-04-28 | Butter of tin process units with wave duct reactor |
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| Publication Number | Publication Date |
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| CN105731530A true CN105731530A (en) | 2016-07-06 |
| CN105731530B CN105731530B (en) | 2017-04-05 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610274775.7A Expired - Fee Related CN105731530B (en) | 2016-04-28 | 2016-04-28 | Butter of tin process units with wave duct reactor |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2061816A (en) * | 1932-05-14 | 1936-11-24 | Gen Chemical Corp | Process of making tin tetrachloride |
| WO1991003425A1 (en) * | 1989-09-04 | 1991-03-21 | Elektro-Chemie Ibbenbüren Gmbh | Process for the continuous production of tin tetrachloride |
| US6001323A (en) * | 1997-09-06 | 1999-12-14 | Vinnolit Monomer Gmbh & Co. Kg | Process for preparing tin tetrachloride |
| CN1958144A (en) * | 2006-09-29 | 2007-05-09 | 浙江大学 | Oscillatory flow tubular reactor with ripple wall |
| CN102180514A (en) * | 2011-03-05 | 2011-09-14 | 招远市松鹤化工有限公司 | Production process of tin tetrachloride |
| CN102580660A (en) * | 2011-01-07 | 2012-07-18 | 丰映科技股份有限公司 | Tubular continuous-type reactor and corrugated-type reactor tube being applied to same |
| CN205575670U (en) * | 2016-04-28 | 2016-09-14 | 南阳师范学院 | Butter of tin apparatus for producing with ripples reactor |
-
2016
- 2016-04-28 CN CN201610274775.7A patent/CN105731530B/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2061816A (en) * | 1932-05-14 | 1936-11-24 | Gen Chemical Corp | Process of making tin tetrachloride |
| WO1991003425A1 (en) * | 1989-09-04 | 1991-03-21 | Elektro-Chemie Ibbenbüren Gmbh | Process for the continuous production of tin tetrachloride |
| US6001323A (en) * | 1997-09-06 | 1999-12-14 | Vinnolit Monomer Gmbh & Co. Kg | Process for preparing tin tetrachloride |
| CN1958144A (en) * | 2006-09-29 | 2007-05-09 | 浙江大学 | Oscillatory flow tubular reactor with ripple wall |
| CN102580660A (en) * | 2011-01-07 | 2012-07-18 | 丰映科技股份有限公司 | Tubular continuous-type reactor and corrugated-type reactor tube being applied to same |
| CN102180514A (en) * | 2011-03-05 | 2011-09-14 | 招远市松鹤化工有限公司 | Production process of tin tetrachloride |
| CN205575670U (en) * | 2016-04-28 | 2016-09-14 | 南阳师范学院 | Butter of tin apparatus for producing with ripples reactor |
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| CN105731530B (en) | 2017-04-05 |
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Granted publication date: 20170405 Termination date: 20200428 |