CN104058406B - A kind of method and device thereof removing aluminum chloride from chlorosilane - Google Patents
A kind of method and device thereof removing aluminum chloride from chlorosilane Download PDFInfo
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- CN104058406B CN104058406B CN201410152511.5A CN201410152511A CN104058406B CN 104058406 B CN104058406 B CN 104058406B CN 201410152511 A CN201410152511 A CN 201410152511A CN 104058406 B CN104058406 B CN 104058406B
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Abstract
The present invention relates to the production field of chlorosilane, be specifically related to a kind of from chlorosilane, remove aluminum chloride method and device thereof, the method specifically comprises the following steps: the chlorosilane containing aluminum chloride is added thermal distillation in the first distillation tower, distillation temperature is 45-65 DEG C, volatile matter is entered removal of impurities in the first trash separator, in the first trash separator, be filled with absorbent particles; Volatile matter after first trash separator removal of impurities is entered second column after filtering and adds thermal distillation, distillation temperature is 180-195 DEG C, volatile matter is entered the second trash separator, is filled with sodium salt particle in the second trash separator; Volatile matter after the second trash separator removal of impurities filters and obtains chlorine purification silane after condenser condenses.This method cost is lower, and removal effect is better, and can not produce degree of depth pollution to chlorosilane.
Description
Technical field
The present invention relates to the production field of chlorosilane, be specifically related to a kind of from chlorosilane, remove aluminum chloride method and device thereof.
Background technology
Chlorosilane is a kind of important Chemicals, and the production cost of chlorosilane is very low, but in their production processes, easily generates halogenide, as aluminum halide.The existence of aluminum halide makes chlorosilane performance during raising temperature very unstable, can chlorosilane be caused to decompose in raising temperature course.In preparation process, impure solid state si and chlorine-containing gas react, and many solid impurities are trapped in this reactor or in the dust removal installation of such as swirler.But the character of aluminium and some other pollutents such as antimony, boron, carbon, indium, gallium, phosphorus, thallium, tin, titanium, zinc and zirconium makes them form volatile compound, is taken out of reactor together with required chlorosilane.Therefore, containing these volatile compounds in the eluting gas of reactor, eluting gas is cooled subsequently forms liquid chlorosilane mixture, and its major ingredient is dichlorosilane (SiH
2cl
2), trichlorosilane (SiHCl
3) and silicon tetrachloride (being also called tetrachloro silicane) (SiCl
4), this mixture mainly adopts distillation to carry out purifying by ordinary method.Aluminium is the same with boron is main impurity, and the two all can be used as the doping agent with electrical activity in high purity silicon, therefore the content of aluminium must be down to extremely low.In addition, because aluminum chloride (AlCl3) has the anomalous property that under atmospheric pressure can not form liquid phase.When pressure close to such as distill normal atmosphere time, aluminum chloride can directly from solid conversion be gas; But aluminum chloride can partly be dissolved in chlorosilane, therefore, although remove aluminum chloride by distillation, but it is very difficult, because often form solid deposited thing in Distallation systm, and can not direct generation high concentration of aluminium liquid waste, therefore need refuse to be processed more, costly and cause environmental problem.
Although someone proposes the method that aluminum halide removes from chlorosilane with the form of complexing aluminum halide by use phosphoryl chloride at present.But, use phosphoryl chloride can not effectively be removed from chlorosilane by aluminum halide, because the complex compound that phosphoryl chloride and aluminum halide are formed shows instability in the decomposition of chlorosilane.When distilling the chlorosilane containing phosphoryl chloride and aluminum halide, partially halogenated aluminium is still stayed in chlorosilane.Meanwhile, phosphoryl chloride effectively can not control the erosion of aluminum halide to chlorosilane when temperature raises, and in addition, the residue of phosphoryl chloride too much also can cause the degree of depth of chlorosilane to be polluted.
There is inefficiency, cost for the removal of aluminum halide in current chlorosilane higher and effectively can not control the problem of chlorosilane quality product, need a kind of method effectively can removing aluminum halide in chlorosilane badly.
Summary of the invention
The object of the invention is to overcome problem described above, providing a kind of from chlorosilane, remove aluminum chloride method and device thereof.
In order to reach foregoing invention object, the present invention by the following technical solutions:
From chlorosilane, remove a method for aluminum chloride, distilled by the chlorosilane containing aluminum chloride, the container of the volatile matter after distillation through being equipped with sodium salt or sylvite reacts and obtains chlorine purification silane after cooling.
as preferably, specifically comprise the following steps:
Chlorosilane containing aluminum chloride is added thermal distillation by a in the first distillation tower, and distillation temperature is 45-65 DEG C, volatile matter is entered removal of impurities in the first trash separator, is filled with absorbent particles in the first trash separator, and sorbent material is ion exchange resin or silica gel;
Volatile matter after step a first trash separator (3) removal of impurities is entered surge tank by b;
The chlorosilane containing impurity in d surge tank (4) enters second column and adds thermal distillation, and distillation temperature is 180-195 DEG C, volatile matter is entered the second trash separator, is filled with sodium salt or sylvite particle in the second trash separator;
The volatile matter of d after the second trash separator removal of impurities filters and obtains chlorine purification silane after condenser condenses.
Someone uses the method that aluminum halide removes from chlorosilane with the form of complexing aluminum halide by phosphoryl chloride at present, but, use the effect of phosphoryl chloride dissatisfied, the complex compound formed due to phosphoryl chloride and aluminum halide shows instability in the decomposition of chlorosilane, when distillation contains the chlorosilane of phosphoryl chloride and aluminum halide, partially halogenated aluminium still distills gasification in the lump with chlorosilane, simultaneously, phosphoryl chloride can not to stop and avoid when temperature raises aluminum halide to the erosion of chlorosilane, residual phosphorus can also cause the degree of depth to pollute to chlorosilane, if phosphorus is clear unclean, can have a negative impact to the performance of chlorosilane.Adopt the aluminum chloride in sodium salt and chlorosilane to carry out complex reaction in the present invention, generate AlCl
3naCl complex compound, and utilize complex compound normal temperature to be solid-state characteristic, being removed by filtering, being reached the object of removing aluminum chloride.
For the sodium salt advantage of lower cost used, even and if residual sodium salt, also can not have a negative impact for chlorosilane.
as preferably, the porosity in the first trash separator is 60-80%.
as preferably, the porosity in the second trash separator is 40-50%.
as preferably, the granularity of the first trash separator internal adsorption agent is 70-150 order, and in the second trash separator, the granularity of sodium salt is 30-160 order.
as preferably, in the first trash separator and the second trash separator, the flow velocity of volatile matter is 0.1-0.15m/s, and volatile matter and sorbent material or sodium salt duration of contact>=10s.The duration of contact of suitable flow velocity and sodium salt and volatile matter accurately can manipulate complex reaction, effectively removes aluminum chloride.
as preferably, first volatile matter carries out preheating to sodium salt or sylvite before contacting with sodium salt or sylvite, and the preheating temperature of sodium salt or sylvite is 180-220 DEG C, and keeps the temperature in the second trash separator to be 180-210 DEG C.
as preferably, the pressure in the first trash separator and the second trash separator is 0.15-0.2Mpa.
as preferably, the sodium salt of described sodium salt or sylvite is one or more of sodium carbonate, sodium sulfate, water glass or sodium-acetate, and described sylvite is one or more of salt of wormwood, potassium sulfate, potassium silicate or Repone K.
A kind of preparation facilities removing the method for aluminum chloride from chlorosilane, comprise stoste storage tank successively, first distillation tower, first trash separator, surge tank, second column, second trash separator, condenser and purification storage tank, stoste storage tank is connected with the first distillation tower bottom, first distillation tower top is connected with the first trash separator, first trash separator is connected with surge tank top, be connected with second column bottom surge tank, second column is connected with the second trash separator top, after-fractionating top of tower is connected with condenser overhead, condenser is connected with purification storage tank, the top of the first trash separator and the second trash separator is equipped with feed pot, bottom is equipped with impurity storage tank, each parts are all connected by pipeline, also strainer is provided with before second column He before purification storage tank.
As preferably, between strainer after the condenser and purification storage tank, be also provided with a rectifying tower.As shown in Figure 2, this rectifying tower can be purified further to chlorosilane.
Compared with prior art, beneficial effect is in the present invention:
1 technique is simple, effectively can remove the aluminum chloride in chlorosilane;
2 avoid current removal aluminum chloride to adopt in the technological process of phosphoryl chloride phosphoryl chloride to the generation of the erosion problem of chlorosilane;
3 avoid in the technological process of current removal aluminum chloride because careless manipulation causes the generation to the problem that the degree of depth of chlorosilane is polluted;
4 removal effects are good, and environmental protection and energy saving, cost is low.
Accompanying drawing explanation
Fig. 1 is the structural representation of the present invention's preparation facilities used;
Fig. 2 is the another kind of structural representation of the present invention's preparation facilities used.
In figure: 1 stoste storage tank, 2 first distillation towers, 3 first trash separators, 4 surge tanks, 5 second columns, 6 second trash separators, 7 condensers, 8 purification storage tanks, 9 feed pots, 10 impurity storage tanks, 11 strainers, 12 rectifying tower.
Embodiment
Below by specific embodiment, explanation is further described to technical scheme of the present invention.
If without specified otherwise, the raw material adopted in embodiments of the invention is the conventional raw material in this area, and the method adopted in embodiment, is the ordinary method of this area.
Embodiment 1:
A kind of preparation facilities removing the method for aluminum chloride from chlorosilane, as shown in Figure 1, comprise stoste storage tank successively, first distillation tower 2, first trash separator 3, surge tank 4, second column 5, second trash separator 6, condenser 7 and purification storage tank 8, stoste storage tank is connected with the first distillation tower 2 bottom, first distillation tower 2 top is connected with the first trash separator 3, first trash separator 3 is connected with surge tank 4 top, be connected with second column 5 bottom surge tank 4, second column 5 is connected with the second trash separator 6 top, second column 5 top is connected with condenser 7 top, condenser 7 is connected with purification storage tank 8, the top of the first trash separator 3 and the second trash separator 6 is equipped with feed pot 9, bottom is equipped with impurity storage tank 10, each parts are all connected by pipeline, strainer 11 is also provided with before second column 5 He before purification storage tank 8.
From chlorosilane, remove a method for aluminum chloride, distilled by the chlorosilane containing aluminum chloride, the container of the volatile matter after distillation through being equipped with sodium salt reacts and obtains chlorine purification silane after cooling, and specifically comprises the following steps:
Chlorosilane containing aluminum chloride is added thermal distillation by a in the first distillation tower 2, distillation temperature is 45-65 DEG C, volatile matter is entered removal of impurities in the first trash separator 3, is filled with absorbent particles in the first trash separator 3, the granularity of sorbent material is 70-150 order, and the porosity in the first trash separator 3 is 60-80%; The flow velocity of volatile matter in the first trash separator 3 is 0.1-0.15m/s, and volatile matter and sorbent material duration of contact >=10s; First will carry out preheating to sodium salt, the preheating temperature of sodium salt is 180-220 DEG C, and keeps the temperature in the first trash separator 36 to be 180-210 DEG C, and the pressure controlled in the first trash separator 3 is 0.15-0.2Mpa;
Volatile matter after the removal of impurities of step a first trash separator 3 is entered surge tank 4 by b;
The chlorosilane containing impurity in c surge tank (4) enters second column 5 and adds thermal distillation, distillation temperature is 180-195 DEG C, volatile matter is entered the second trash separator 6, sodium salt particle is filled with in second trash separator 6, the granularity of sodium salt is 30-160 order, porosity in second trash separator 6 is 40-50%, and the flow velocity of volatile matter in the second trash separator 3 is 0.1-0.15m/s, and volatile matter and sodium salt duration of contact >=10s; First will carry out preheating to sodium salt, the preheating temperature of sodium salt is 180-220 DEG C, and keeps the temperature in the second trash separator 6 to be 180-210 DEG C, and the pressure controlled in the second trash separator 6 is 0.15-0.2Mpa;
The volatile matter of d after the second trash separator 6 removal of impurities obtains chlorine purification silane after condenser 7 condensation.
Embodiment 2:
A kind of preparation facilities removing the method for aluminum chloride from chlorosilane, as shown in Figure 1, comprise stoste storage tank successively, first distillation tower 2, first trash separator 3, surge tank 4, second column 5, second trash separator 6, condenser 7 and purification storage tank 8, stoste storage tank is connected with the first distillation tower 2 bottom, first distillation tower 2 top is connected with the first trash separator 3, first trash separator 3 is connected with surge tank 4 top, be connected with second column 5 bottom surge tank 4, second column 5 is connected with the second trash separator 6 top, second column 5 top is connected with condenser 7 top, condenser 7 is connected with purification storage tank 8, the top of the first trash separator 3 and the second trash separator 6 is equipped with feed pot 9, bottom is equipped with impurity storage tank 10, each parts are all connected by pipeline, strainer 11 is also provided with before second column 5 He before purification storage tank 8.
From chlorosilane, remove a method for aluminum chloride, distilled by the chlorosilane containing aluminum chloride, the container of the volatile matter after distillation through being equipped with sodium salt reacts and obtains chlorine purification silane after cooling, and specifically comprises the following steps:
A is the content of aluminum chloride in chlorine detection silane first, then in chlorosilane, add the sodium salt with aluminum chloride mass percent 110%, and then the chlorosilane containing aluminum chloride and sodium salt is added thermal distillation in the first distillation tower 2, distillation temperature is 45 DEG C, volatile matter is entered removal of impurities in the first trash separator 3, be filled with absorbent particles in first trash separator 3, the granularity of sorbent material is 150 orders, and the porosity in the first trash separator 3 is 60%; The flow velocity of volatile matter in the first trash separator 3 is 0.15m/s, and volatile matter and sodium salt duration of contact >=10s; First will carry out preheating to sodium salt, the preheating temperature of sodium salt is 180 DEG C, and keeps the temperature in the first trash separator 36 to be 210 DEG C, and the pressure controlled in the first trash separator 3 is 0.15Mpa;
Volatile matter after the removal of impurities of step a first trash separator 3 is entered surge tank 4 by b;
The chlorosilane containing impurity in c surge tank (4) enters second column 5 and adds thermal distillation, distillation temperature is 195 DEG C, volatile matter is entered the second trash separator 6, sodium salt particle is filled with in second trash separator 6, the granularity of sodium salt is 30 orders, porosity in second trash separator 6 is 50%, and the flow velocity of volatile matter in the second trash separator 3 is 0.1m/s, and volatile matter and sodium salt duration of contact >=10s; First will carry out preheating to sodium salt, the preheating temperature of sodium salt is 220 DEG C, and keeps the temperature in the second trash separator 6 to be 180 DEG C, and the pressure controlled in the second trash separator 6 is 0.2Mpa;
The volatile matter of d after the second trash separator 6 removal of impurities after condenser 7 condensation is filtered, and then obtains chlorine purification silane through rectifying.
Embodiment 3:
A kind of preparation facilities removing the method for aluminum chloride from chlorosilane, as shown in Figure 1, comprise stoste storage tank successively, first distillation tower 2, first trash separator 3, surge tank 4, second column 5, second trash separator 6, condenser 7 and purification storage tank 8, stoste storage tank is connected with the first distillation tower 2 bottom, first distillation tower 2 top is connected with the first trash separator 3, first trash separator 3 is connected with surge tank 4 top, be connected with second column 5 bottom surge tank 4, second column 5 is connected with the second trash separator 6 top, second column 5 top is connected with condenser 7 top, condenser 7 is connected with purification storage tank 8, the top of the first trash separator 3 and the second trash separator 6 is equipped with feed pot 9, bottom is equipped with impurity storage tank 10, each parts are all connected by pipeline, strainer 11 is also provided with before second column 5 He before purification storage tank 8.
From chlorosilane, remove a method for aluminum chloride, distilled by the chlorosilane containing aluminum chloride, the container of the volatile matter after distillation through being equipped with sodium salt reacts and obtains chlorine purification silane after cooling, and specifically comprises the following steps:
A is the content of aluminum chloride in chlorine detection silane first, then in chlorosilane, add the sodium salt with aluminum chloride mass percent 90%, and then the chlorosilane containing aluminum chloride and sodium salt is added thermal distillation in the first distillation tower 2, distillation temperature is 65 DEG C, volatile matter is entered removal of impurities in the first trash separator 3, be filled with absorbent particles in first trash separator 3, the granularity of sorbent material is 70 orders, and the porosity in the first trash separator 3 is 80%; The flow velocity of volatile matter in the first trash separator 3 is 0.1m/s, and volatile matter and sodium salt duration of contact >=10s; First will carry out preheating to sodium salt, the preheating temperature of sodium salt is 220 DEG C, and keeps the temperature in the first trash separator 36 to be 180 DEG C, and the pressure controlled in the first trash separator 3 is 0.2Mpa;
Volatile matter after the removal of impurities of step a first trash separator 3 is entered surge tank 4 by b;
The chlorosilane containing impurity in c surge tank (4) enters second column 5 and adds thermal distillation, distillation temperature is 180 DEG C, volatile matter is entered the second trash separator 6, sodium salt particle is filled with in second trash separator 6, the granularity of sodium salt is 160 orders, porosity in second trash separator 6 is 40%, and the flow velocity of volatile matter in the second trash separator 3 is 0.15m/s, and volatile matter and sodium salt duration of contact >=10s; First will carry out preheating to sodium salt, the preheating temperature of sodium salt is 180 DEG C, and keeps the temperature in the second trash separator 6 to be 210 DEG C, and the pressure controlled in the second trash separator 6 is 0.15Mpa;
The volatile matter of d after the second trash separator 6 removal of impurities obtains chlorine purification silane after condenser 7 condensation.
In the scheme of embodiment 1-3, sodium salt is individually tested with sodium carbonate, sodium sulfate, water glass and sodium-acetate respectively, and then with testing between two in sodium carbonate, sodium sulfate, water glass or sodium-acetate.
Embodiment 4:
A kind of preparation facilities removing the method for aluminum chloride from chlorosilane, as shown in Figure 1, comprise stoste storage tank successively, first distillation tower 2, first trash separator 3, surge tank 4, second column 5, second trash separator 6, condenser 7 and purification storage tank 8, stoste storage tank is connected with the first distillation tower 2 bottom, first distillation tower 2 top is connected with the first trash separator 3, first trash separator 3 is connected with surge tank 4 top, be connected with second column 5 bottom surge tank 4, second column 5 is connected with the second trash separator 6 top, second column 5 top is connected with condenser 7 top, condenser 7 is connected with purification storage tank 8, the top of the first trash separator 3 and the second trash separator 6 is equipped with feed pot 9, bottom is equipped with impurity storage tank 10, each parts are all connected by pipeline, strainer 11 is also provided with before second column 5 He before purification storage tank 8.
From chlorosilane, remove a method for aluminum chloride, distilled by the chlorosilane containing aluminum chloride, the container of the volatile matter after distillation through being equipped with sylvite reacts and obtains chlorine purification silane after cooling, and specifically comprises the following steps:
Chlorosilane containing aluminum chloride is added thermal distillation by a in the first distillation tower 2, distillation temperature is 45-65 DEG C, volatile matter is entered removal of impurities in the first trash separator 3, is filled with absorbent particles in the first trash separator 3, the granularity of sorbent material is 70-150 order, and the porosity in the first trash separator 3 is 60-80%; The flow velocity of volatile matter in the first trash separator 3 is 0.1-0.15m/s, and volatile matter and sorbent material duration of contact >=10s; First will carry out preheating to sylvite, the preheating temperature of sylvite is 180-220 DEG C, and keeps the temperature in the first trash separator 36 to be 180-210 DEG C, and the pressure controlled in the first trash separator 3 is 0.15-0.2Mpa;
Volatile matter after the removal of impurities of step a first trash separator 3 is entered surge tank 4 by b;
The chlorosilane containing impurity in c surge tank (4) enters second column 5 and adds thermal distillation, distillation temperature is 180-195 DEG C, volatile matter is entered the second trash separator 6, sylvite particle is filled with in second trash separator 6, the granularity of sylvite is 30-160 order, porosity in second trash separator 6 is 40-50%, and the flow velocity of volatile matter in the second trash separator 3 is 0.1-0.15m/s, and volatile matter and sylvite duration of contact >=10s; First will carry out preheating to sylvite, the preheating temperature of sylvite is 180-220 DEG C, and keeps the temperature in the second trash separator 6 to be 180-210 DEG C, and the pressure controlled in the second trash separator 6 is 0.15-0.2Mpa;
The volatile matter of d after the second trash separator 6 removal of impurities obtains chlorine purification silane after condenser 7 condensation.
Embodiment 5:
A kind of preparation facilities removing the method for aluminum chloride from chlorosilane, as shown in Figure 1, comprise stoste storage tank successively, first distillation tower 2, first trash separator 3, surge tank 4, second column 5, second trash separator 6, condenser 7 and purification storage tank 8, stoste storage tank is connected with the first distillation tower 2 bottom, first distillation tower 2 top is connected with the first trash separator 3, first trash separator 3 is connected with surge tank 4 top, be connected with second column 5 bottom surge tank 4, second column 5 is connected with the second trash separator 6 top, second column 5 top is connected with condenser 7 top, condenser 7 is connected with purification storage tank 8, the top of the first trash separator 3 and the second trash separator 6 is equipped with feed pot 9, bottom is equipped with impurity storage tank 10, each parts are all connected by pipeline, strainer 11 is also provided with before second column 5 He before purification storage tank 8.
From chlorosilane, remove a method for aluminum chloride, distilled by the chlorosilane containing aluminum chloride, the container of the volatile matter after distillation through being equipped with sylvite reacts and obtains chlorine purification silane after cooling, and specifically comprises the following steps:
A is the content of aluminum chloride in chlorine detection silane first, then in chlorosilane, add the sylvite with aluminum chloride mass percent 110%, and then the chlorosilane containing aluminum chloride and sylvite is added thermal distillation in the first distillation tower 2, distillation temperature is 45 DEG C, volatile matter is entered removal of impurities in the first trash separator 3, be filled with absorbent particles in first trash separator 3, the granularity of sorbent material is 150 orders, and the porosity in the first trash separator 3 is 60%; The flow velocity of volatile matter in the first trash separator 3 is 0.15m/s, and volatile matter and sylvite duration of contact >=10s; First will carry out preheating to sylvite, the preheating temperature of sylvite is 180 DEG C, and keeps the temperature in the first trash separator 36 to be 210 DEG C, and the pressure controlled in the first trash separator 3 is 0.15Mpa;
Volatile matter after the removal of impurities of step a first trash separator 3 is entered surge tank 4 by b;
The chlorosilane containing impurity in c surge tank (4) enters second column 5 and adds thermal distillation, distillation temperature is 195 DEG C, volatile matter is entered the second trash separator 6, sylvite particle is filled with in second trash separator 6, the granularity of sylvite is 30 orders, porosity in second trash separator 6 is 50%, and the flow velocity of volatile matter in the second trash separator 3 is 0.1m/s, and volatile matter and sylvite duration of contact >=10s; First will carry out preheating to sylvite, the preheating temperature of sylvite is 220 DEG C, and keeps the temperature in the second trash separator 6 to be 180 DEG C, and the pressure controlled in the second trash separator 6 is 0.2Mpa;
The volatile matter of d after the second trash separator 6 removal of impurities after condenser 7 condensation is filtered, and then obtains chlorine purification silane through rectifying.
Embodiment 6:
A kind of preparation facilities removing the method for aluminum chloride from chlorosilane, as shown in Figure 1, comprise stoste storage tank successively, first distillation tower 2, first trash separator 3, surge tank 4, second column 5, second trash separator 6, condenser 7 and purification storage tank 8, stoste storage tank is connected with the first distillation tower 2 bottom, first distillation tower 2 top is connected with the first trash separator 3, first trash separator 3 is connected with surge tank 4 top, be connected with second column 5 bottom surge tank 4, second column 5 is connected with the second trash separator 6 top, second column 5 top is connected with condenser 7 top, condenser 7 is connected with purification storage tank 8, the top of the first trash separator 3 and the second trash separator 6 is equipped with feed pot 9, bottom is equipped with impurity storage tank 10, each parts are all connected by pipeline, strainer 11 is also provided with before second column 5 He before purification storage tank 8.
From chlorosilane, remove a method for aluminum chloride, distilled by the chlorosilane containing aluminum chloride, the container of the volatile matter after distillation through being equipped with sylvite reacts and obtains chlorine purification silane after cooling, and specifically comprises the following steps:
A is the content of aluminum chloride in chlorine detection silane first, then in chlorosilane, add the sylvite with aluminum chloride mass percent 90%, and then the chlorosilane containing aluminum chloride and sylvite is added thermal distillation in the first distillation tower 2, distillation temperature is 65 DEG C, volatile matter is entered removal of impurities in the first trash separator 3, be filled with absorbent particles in first trash separator 3, the granularity of sorbent material is 70 orders, and the porosity in the first trash separator 3 is 80%; The flow velocity of volatile matter in the first trash separator 3 is 0.1m/s, and volatile matter and sylvite duration of contact >=10s; First will carry out preheating to sylvite, the preheating temperature of sylvite is 220 DEG C, and keeps the temperature in the first trash separator 36 to be 180 DEG C, and the pressure controlled in the first trash separator 3 is 0.2Mpa;
Volatile matter after the removal of impurities of step a first trash separator 3 is entered surge tank 4 by b;
The chlorosilane containing impurity in c surge tank (4) enters second column 5 and adds thermal distillation, distillation temperature is 180 DEG C, volatile matter is entered the second trash separator 6, sylvite particle is filled with in second trash separator 6, the granularity of sylvite is 160 orders, porosity in second trash separator 6 is 40%, and the flow velocity of volatile matter in the second trash separator 3 is 0.15m/s, and volatile matter and sylvite duration of contact >=10s; First will carry out preheating to sylvite, the preheating temperature of sylvite is 180 DEG C, and keeps the temperature in the second trash separator 6 to be 210 DEG C, and the pressure controlled in the second trash separator 6 is 0.15Mpa;
The volatile matter of d after the second trash separator 6 removal of impurities obtains chlorine purification silane after condenser 7 condensation.
In the scheme of embodiment 4-6, sylvite is tested respectively with salt of wormwood, potassium sulfate, potassium silicate and Repone K respectively, and then with testing between two in salt of wormwood, potassium sulfate, potassium silicate or Repone K.
Claims (9)
1. from chlorosilane, remove a method for aluminum chloride, it is characterized in that, distilled by the chlorosilane containing aluminum chloride, the container of the volatile matter after distillation through being equipped with sodium salt or sylvite reacts and obtains chlorine purification silane after cooling;
Specifically comprise the following steps:
Chlorosilane containing aluminum chloride is added thermal distillation by a in the first distillation tower (2), and distillation temperature is 45-65 DEG C, volatile matter is entered the first trash separator (3) interior removal of impurities, and the first trash separator is filled with sorbent material in (3);
Volatile matter after step a first trash separator (3) removal of impurities is entered surge tank (4) by b;
The chlorosilane containing impurity in c surge tank (4) enters second column (5) and adds thermal distillation, and distillation temperature is 180-195 DEG C, volatile matter is entered the second trash separator (6), is filled with sodium salt or sylvite particle in the second trash separator (6);
The volatile matter of d after the second trash separator (6) removal of impurities obtains chlorine purification silane after condenser (7) condensation is filtered.
2. a kind of method removing aluminum chloride from chlorosilane according to claim 1, is characterized in that, the porosity in the first trash separator (3) is 60-80%, and the porosity in the second trash separator (6) is 40-50%.
3. a kind of method removing aluminum chloride from chlorosilane according to claim 1, is characterized in that, the granularity of the first trash separator (3) internal adsorption agent is 70-150 order, and in the second trash separator (6), the granularity of sodium salt or sylvite is 30-160 order.
4. a kind of method removing aluminum chloride from chlorosilane according to claim 1, it is characterized in that, in first trash separator (3) and the second trash separator (6), the flow velocity of volatile matter is 0.1-0.15m/s, and volatile matter and sorbent material or sodium salt or sylvite duration of contact >=10s.
5. a kind of method removing aluminum chloride from chlorosilane according to claim 1, is characterized in that, first adds and the sodium salt of aluminum chloride mass percent 90%-110% or sylvite in containing the chlorosilane of aluminum chloride before step a distillation.
6. a kind of method removing aluminum chloride from chlorosilane according to claim 1, it is characterized in that, first volatile matter carries out preheating to sodium salt or sylvite before contacting with sodium salt or sylvite, the preheating temperature of sodium salt or sylvite is 180-220 DEG C, and keeps the temperature in the second trash separator (6) to be 180-210 DEG C.
7. a kind of method removing aluminum chloride from chlorosilane according to claim 1, is characterized in that, the pressure in the first trash separator (3) and the second trash separator (6) is 0.15-0.2Mpa.
8. a kind of method removing aluminum chloride from chlorosilane according to claim 1, it is characterized in that, sodium salt in described sodium salt or sylvite is one or more of sodium carbonate, water glass or sodium-acetate, and described sylvite is one or more of salt of wormwood, potassium silicate or Repone K.
9. one kind for a kind of device removing the method for aluminum chloride from chlorosilane according to claim 1, it is characterized in that, comprise stoste storage tank (1) successively, first distillation tower (2), first trash separator (3), surge tank (4), second column (5), second trash separator (6), condenser (7) and purification storage tank (8), stoste storage tank is connected with the first distillation tower (2) bottom, first distillation tower (2) top is connected with the first trash separator (3), first trash separator (3) is connected with surge tank (4) top, surge tank (4) bottom is connected with second column (5), second column (5) is connected with the second trash separator (6) top, second column (5) top is connected with condenser (7) top, condenser (7) is connected with purification storage tank (8), the top of the first trash separator (3) and the second trash separator (6) is equipped with sodium salt or sylvite feed pot (9), bottom is equipped with impurity storage tank (10), each parts are all connected by pipeline, second column (5) is front and purification storage tank (8) is front is also provided with strainer (11).
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410152511.5A CN104058406B (en) | 2014-04-15 | 2014-04-15 | A kind of method and device thereof removing aluminum chloride from chlorosilane |
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| CN201410152511.5A CN104058406B (en) | 2014-04-15 | 2014-04-15 | A kind of method and device thereof removing aluminum chloride from chlorosilane |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101544373A (en) * | 2008-03-24 | 2009-09-30 | 三菱麻铁里亚尔株式会社 | Chlorosilanes purifying apparatus and chlorosilanes purifying method |
| CN202315386U (en) * | 2011-11-21 | 2012-07-11 | 江苏弘博新材料有限公司 | Device for separating gaseous methyl chlorosilane and aluminum chloride |
| CN202620940U (en) * | 2012-04-09 | 2012-12-26 | 南京合创化工工程有限公司 | Complete device for removing aluminum chloride heavy metal impurities in cold hydrogenation tail gas |
| CN103553122A (en) * | 2013-11-14 | 2014-02-05 | 攀枝花钢企欣宇化工有限公司 | Method for removing aluminum trichloride from chlorination system for producing titanium tetrachloride |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101544373A (en) * | 2008-03-24 | 2009-09-30 | 三菱麻铁里亚尔株式会社 | Chlorosilanes purifying apparatus and chlorosilanes purifying method |
| CN202315386U (en) * | 2011-11-21 | 2012-07-11 | 江苏弘博新材料有限公司 | Device for separating gaseous methyl chlorosilane and aluminum chloride |
| CN202620940U (en) * | 2012-04-09 | 2012-12-26 | 南京合创化工工程有限公司 | Complete device for removing aluminum chloride heavy metal impurities in cold hydrogenation tail gas |
| CN103553122A (en) * | 2013-11-14 | 2014-02-05 | 攀枝花钢企欣宇化工有限公司 | Method for removing aluminum trichloride from chlorination system for producing titanium tetrachloride |
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