CN104058406A - Method and device for removing aluminum trichloride from chlorosilane - Google Patents
Method and device for removing aluminum trichloride from chlorosilane Download PDFInfo
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- CN104058406A CN104058406A CN201410152511.5A CN201410152511A CN104058406A CN 104058406 A CN104058406 A CN 104058406A CN 201410152511 A CN201410152511 A CN 201410152511A CN 104058406 A CN104058406 A CN 104058406A
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Abstract
The invention relates to the field of production of chlorosilane, and particularly relates to a method and a device for removing aluminum trichloride from the chlorosilane. The method concretely comprises the following steps: heating and distilling the chlorosilane which contains aluminum trichloride in a first distillation tower at a distillation temperature of 45-65 DEG C, and entering volatile matters into a first impurity remover for removing impurities, wherein the first impurity remover is filled with adsorbent particles; filtering the volatile matters from which the impurities are removed by the first impurity remover and then heating and distilling the volatile matters in a second impurity remover at the distillation temperature of 180-195 DEG C, and entering the volatile matters into the second impurity remover which is filled with sodium salt particles; condensing the volatile matters from which the impurities are removed by the second impurity remover by use of a condenser and then filtering to obtain purified chlorosilane. The method is low in cost and good in removal effect, and also causes no deep pollution to the chlorosilane.
Description
Technical field
The present invention relates to the production field of chlorosilane, be specifically related to a kind of method and device thereof of removing aluminum chloride from chlorosilane.
Background technology
Chlorosilane is a kind of important Chemicals, and the production cost of chlorosilane is very low, but easily generates halogenide in their production processes, as aluminum halide.Chlorosilane performance when the existence of aluminum halide makes to improve temperature is very unstable, can in raising temperature course, cause chlorosilane to decompose.In preparation process, impure solid state si is reacted with chlorine-containing gas, and many solid impurities are trapped in the dust removal installation in this reactor or such as swirler.But aluminium and for example character of antimony, boron, carbon, indium, gallium, phosphorus, thallium, tin, titanium, zinc and zirconium of some other pollutents make them form volatile compound, are taken out of reactor together with needed chlorosilane.Therefore, contain these volatile compounds in the eluting gas of reactor, eluting gas is cooled subsequently and 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 can mainly adopt 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 approach for example for distill normal atmosphere time, aluminum chloride can directly be converted into gas from solid; But aluminum chloride can partly be dissolved in chlorosilane, therefore, although can remove aluminum chloride by distillation, but very difficult, because tend to form solid deposited thing in Distallation systm, and can not be directly 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 uses phosphoryl chloride that aluminum halide is removed from chlorosilane with the form of complexing aluminum halide at present.But, use phosphoryl chloride effectively aluminum halide not to be removed from chlorosilane, because the complex compound that phosphoryl chloride and aluminum halide form shows unstable in the decomposition of chlorosilane.When contain phosphoryl chloride and aluminum halide in distillation chlorosilane time, partially halogenated aluminium is still stayed in chlorosilane.Meanwhile, phosphoryl chloride can not effectively be controlled the erosion of aluminum halide to chlorosilane in the time that temperature raises, and in addition, the residue of phosphoryl chloride too much also can cause the degree of depth of chlorosilane to be polluted.
Exist inefficiency, cost higher and can not effectively control the problem of chlorosilane quality product for the removal of aluminum halide in current chlorosilane, need a kind of method that can effectively remove aluminum halide in chlorosilane badly.
Summary of the invention
The object of the invention is in order to overcome problem described above, a kind of method and device thereof of removing aluminum chloride from chlorosilane is provided.
In order to reach foregoing invention object, the present invention by the following technical solutions:
From chlorosilane, remove a method for aluminum chloride, the chlorosilane that contains aluminum chloride distilled, the volatile matter after distillation through be equipped with sodium salt or sylvite container reaction and cooling after obtain chlorine purification silane.
as preferably, specifically comprise the following steps:
A adds thermal distillation by the chlorosilane that contains aluminum chloride in the first distillation tower, and distillation temperature is 45-65 DEG C, and volatile matter is entered to removal of impurities in the first trash separator, in the first trash separator, is filled with absorbent particles, and sorbent material is ion exchange resin or silica gel;
The volatile matter after step a the first trash separator (3) removal of impurities is entered surge tank by b;
The chlorosilane that contains impurity in d surge tank (4) enters second column and adds thermal distillation, and distillation temperature is 180-195 DEG C, and volatile matter is entered to 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 phosphoryl chloride removes with the form of complexing aluminum halide aluminum halide from chlorosilane at present, but, use the effect of phosphoryl chloride dissatisfied, because the complex compound of phosphoryl chloride and aluminum halide formation shows unstable in the decomposition of chlorosilane, the chlorosilane that contains phosphoryl chloride and aluminum halide when distillation, partially halogenated aluminium still distills gasification in the lump with chlorosilane, simultaneously, phosphoryl chloride can not stop and avoid the erosion of aluminum halide to chlorosilane in the time that temperature raises, 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.In the present invention, adopt the aluminum chloride in sodium salt and chlorosilane to carry out complex reaction, generate AlCl
3naCl complex compound, and to utilize complex compound normal temperature be solid-state characteristic, removed by filtering, and reaches the object of removing aluminum chloride.
Relatively low for the sodium salt cost using, even and 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, 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 the duration of contact>=10s of volatile matter and sorbent material or sodium salt.Can accurately manipulate the duration of contact of suitable flow velocity and sodium salt and volatile matter to 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 to keep the temperature in the second trash separator 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, described sylvite is one or more of salt of wormwood, potassium sulfate, potassium silicate or Repone K.
A kind of preparation facilities of the method for removing aluminum chloride from chlorosilane, comprise successively former liquid storage tank, the first distillation tower, the first trash separator, surge tank, second column, the second trash separator, condenser and purification storage tank, former liquid storage tank is connected with the first distillation tower bottom, the first distillation tower top is connected with the first trash separator, the first trash separator is connected with surge tank top, surge tank bottom is connected with second column, 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 all connect by pipeline, before second column He before purification storage tank, be also provided with strainer.
As preferably, between the strainer after condenser and purification storage tank, be also provided with a rectifying tower.As shown in Figure 2, this rectifying tower can further be purified to chlorosilane.
Compared with prior art, beneficial effect is in the present invention:
1 technique is simple, can effectively remove the aluminum chloride in chlorosilane;
2 have avoided current removal aluminum chloride to adopt the generation of the erosion problem of phosphoryl chloride to chlorosilane in the technological process of phosphoryl chloride;
3 avoid causing due to careless manipulation in the technological process of current removal aluminum chloride the generation of the problem that the degree of depth of chlorosilane is polluted;
4 removal effects are good, and environmental protection and energy saving, and cost is low.
Brief description of the drawings
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 former liquid 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, technical scheme of the present invention is further described to explanation.
If without specified otherwise, the raw material adopting in embodiments of the invention is the conventional raw material in this area, and the method adopting in embodiment is the ordinary method of this area.
Embodiment 1:
A kind of preparation facilities of the method for removing aluminum chloride from chlorosilane, as shown in Figure 1, comprise successively former liquid storage tank, the first distillation tower 2, the first trash separator 3, surge tank 4, second column 5, the second trash separator 6, condenser 7 and purification storage tank 8, former liquid storage tank is connected with the first distillation tower 2 bottoms, the first distillation tower 2 tops are connected with the first trash separator 3, the first trash separator 3 is connected with surge tank 4 tops, surge tank 4 bottoms are connected with second column 5, second column 5 is connected with the second trash separator 6 tops, second column 5 tops are connected with condenser 7 tops, 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 all connect by pipeline, before second column 5 He before purification storage tank 8, be also provided with strainer 11.
From chlorosilane, remove a method for aluminum chloride, the chlorosilane that contains aluminum chloride distilled, the volatile matter after distillation through be equipped with sodium salt container reaction and cooling after obtain chlorine purification silane, specifically comprise the following steps:
A adds thermal distillation by the chlorosilane that contains aluminum chloride in the first distillation tower 2, distillation temperature is 45-65 DEG C, and volatile matter is entered to the interior removal of impurities of the first trash separator 3, in the first trash separator 3, is filled with absorbent particles, 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 the duration of contact >=10s of volatile matter and sorbent material; First will carry out preheating to sodium salt, the preheating temperature of sodium salt is 180-220 DEG C, and to keep the temperature in the first trash separator 36 be 180-210 DEG C, and the pressure of controlling in the first trash separator 3 is 0.15-0.2Mpa;
The volatile matter after step a the first trash separator 3 removal of impurities is entered surge tank 4 by b;
The chlorosilane that contains 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 to the second trash separator 6, in the second trash separator 6, be filled with sodium salt particle, the granularity of sodium salt is 30-160 order, porosity in the 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 to keep the temperature in the second trash separator 6 be 180-210 DEG C, and the pressure of controlling 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 condensations.
Embodiment 2:
A kind of preparation facilities of the method for removing aluminum chloride from chlorosilane, as shown in Figure 1, comprise successively former liquid storage tank, the first distillation tower 2, the first trash separator 3, surge tank 4, second column 5, the second trash separator 6, condenser 7 and purification storage tank 8, former liquid storage tank is connected with the first distillation tower 2 bottoms, the first distillation tower 2 tops are connected with the first trash separator 3, the first trash separator 3 is connected with surge tank 4 tops, surge tank 4 bottoms are connected with second column 5, second column 5 is connected with the second trash separator 6 tops, second column 5 tops are connected with condenser 7 tops, 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 all connect by pipeline, before second column 5 He before purification storage tank 8, be also provided with strainer 11.
From chlorosilane, remove a method for aluminum chloride, the chlorosilane that contains aluminum chloride distilled, the volatile matter after distillation through be equipped with sodium salt container reaction and cooling after obtain chlorine purification silane, specifically comprise 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 that contains aluminum chloride and sodium salt is added to thermal distillation in the first distillation tower 2, distillation temperature is 45 DEG C, volatile matter is entered to the interior removal of impurities of the first trash separator 3, in the first trash separator 3, be filled with absorbent particles, 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 to keep the temperature in the first trash separator 36 be 210 DEG C, and the pressure of controlling in the first trash separator 3 is 0.15Mpa;
The volatile matter after step a the first trash separator 3 removal of impurities is entered surge tank 4 by b;
The chlorosilane that contains impurity in c surge tank (4) enters second column 5 and adds thermal distillation, distillation temperature is 195 DEG C, volatile matter is entered to the second trash separator 6, in the second trash separator 6, be filled with sodium salt particle, the granularity of sodium salt is 30 orders, porosity in the 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 to keep the temperature in the second trash separator 6 be 180 DEG C, and the pressure of controlling 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 condensations are filtered, and then obtains chlorine purification silane through rectifying.
Embodiment 3:
A kind of preparation facilities of the method for removing aluminum chloride from chlorosilane, as shown in Figure 1, comprise successively former liquid storage tank, the first distillation tower 2, the first trash separator 3, surge tank 4, second column 5, the second trash separator 6, condenser 7 and purification storage tank 8, former liquid storage tank is connected with the first distillation tower 2 bottoms, the first distillation tower 2 tops are connected with the first trash separator 3, the first trash separator 3 is connected with surge tank 4 tops, surge tank 4 bottoms are connected with second column 5, second column 5 is connected with the second trash separator 6 tops, second column 5 tops are connected with condenser 7 tops, 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 all connect by pipeline, before second column 5 He before purification storage tank 8, be also provided with strainer 11.
From chlorosilane, remove a method for aluminum chloride, the chlorosilane that contains aluminum chloride distilled, the volatile matter after distillation through be equipped with sodium salt container reaction and cooling after obtain chlorine purification silane, specifically comprise 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 that contains aluminum chloride and sodium salt is added to thermal distillation in the first distillation tower 2, distillation temperature is 65 DEG C, volatile matter is entered to the interior removal of impurities of the first trash separator 3, in the first trash separator 3, be filled with absorbent particles, 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 to keep the temperature in the first trash separator 36 be 180 DEG C, and the pressure of controlling in the first trash separator 3 is 0.2Mpa;
The volatile matter after step a the first trash separator 3 removal of impurities is entered surge tank 4 by b;
The chlorosilane that contains impurity in c surge tank (4) enters second column 5 and adds thermal distillation, distillation temperature is 180 DEG C, volatile matter is entered to the second trash separator 6, in the second trash separator 6, be filled with sodium salt particle, the granularity of sodium salt is 160 orders, porosity in the 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 to keep the temperature in the second trash separator 6 be 210 DEG C, and the pressure of controlling 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 condensations.
In the scheme of embodiment 1-3, sodium salt is tested separately respectively 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 of the method for removing aluminum chloride from chlorosilane, as shown in Figure 1, comprise successively former liquid storage tank, the first distillation tower 2, the first trash separator 3, surge tank 4, second column 5, the second trash separator 6, condenser 7 and purification storage tank 8, former liquid storage tank is connected with the first distillation tower 2 bottoms, the first distillation tower 2 tops are connected with the first trash separator 3, the first trash separator 3 is connected with surge tank 4 tops, surge tank 4 bottoms are connected with second column 5, second column 5 is connected with the second trash separator 6 tops, second column 5 tops are connected with condenser 7 tops, 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 all connect by pipeline, before second column 5 He before purification storage tank 8, be also provided with strainer 11.
From chlorosilane, remove a method for aluminum chloride, the chlorosilane that contains aluminum chloride distilled, the volatile matter after distillation through be equipped with sylvite container reaction and cooling after obtain chlorine purification silane, specifically comprise the following steps:
A adds thermal distillation by the chlorosilane that contains aluminum chloride in the first distillation tower 2, distillation temperature is 45-65 DEG C, and volatile matter is entered to the interior removal of impurities of the first trash separator 3, in the first trash separator 3, is filled with absorbent particles, 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 the duration of contact >=10s of volatile matter and sorbent material; First will carry out preheating to sylvite, the preheating temperature of sylvite is 180-220 DEG C, and to keep the temperature in the first trash separator 36 be 180-210 DEG C, and the pressure of controlling in the first trash separator 3 is 0.15-0.2Mpa;
The volatile matter after step a the first trash separator 3 removal of impurities is entered surge tank 4 by b;
The chlorosilane that contains 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 to the second trash separator 6, in the second trash separator 6, be filled with sylvite particle, the granularity of sylvite is 30-160 order, porosity in the 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 to keep the temperature in the second trash separator 6 be 180-210 DEG C, and the pressure of controlling 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 condensations.
Embodiment 5:
A kind of preparation facilities of the method for removing aluminum chloride from chlorosilane, as shown in Figure 1, comprise successively former liquid storage tank, the first distillation tower 2, the first trash separator 3, surge tank 4, second column 5, the second trash separator 6, condenser 7 and purification storage tank 8, former liquid storage tank is connected with the first distillation tower 2 bottoms, the first distillation tower 2 tops are connected with the first trash separator 3, the first trash separator 3 is connected with surge tank 4 tops, surge tank 4 bottoms are connected with second column 5, second column 5 is connected with the second trash separator 6 tops, second column 5 tops are connected with condenser 7 tops, 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 all connect by pipeline, before second column 5 He before purification storage tank 8, be also provided with strainer 11.
From chlorosilane, remove a method for aluminum chloride, the chlorosilane that contains aluminum chloride distilled, the volatile matter after distillation through be equipped with sylvite container reaction and cooling after obtain chlorine purification silane, specifically comprise 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 that contains aluminum chloride and sylvite is added to thermal distillation in the first distillation tower 2, distillation temperature is 45 DEG C, volatile matter is entered to the interior removal of impurities of the first trash separator 3, in the first trash separator 3, be filled with absorbent particles, 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 to keep the temperature in the first trash separator 36 be 210 DEG C, and the pressure of controlling in the first trash separator 3 is 0.15Mpa;
The volatile matter after step a the first trash separator 3 removal of impurities is entered surge tank 4 by b;
The chlorosilane that contains impurity in c surge tank (4) enters second column 5 and adds thermal distillation, distillation temperature is 195 DEG C, volatile matter is entered to the second trash separator 6, in the second trash separator 6, be filled with sylvite particle, the granularity of sylvite is 30 orders, porosity in the 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 to keep the temperature in the second trash separator 6 be 180 DEG C, and the pressure of controlling 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 condensations are filtered, and then obtains chlorine purification silane through rectifying.
Embodiment 6:
A kind of preparation facilities of the method for removing aluminum chloride from chlorosilane, as shown in Figure 1, comprise successively former liquid storage tank, the first distillation tower 2, the first trash separator 3, surge tank 4, second column 5, the second trash separator 6, condenser 7 and purification storage tank 8, former liquid storage tank is connected with the first distillation tower 2 bottoms, the first distillation tower 2 tops are connected with the first trash separator 3, the first trash separator 3 is connected with surge tank 4 tops, surge tank 4 bottoms are connected with second column 5, second column 5 is connected with the second trash separator 6 tops, second column 5 tops are connected with condenser 7 tops, 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 all connect by pipeline, before second column 5 He before purification storage tank 8, be also provided with strainer 11.
From chlorosilane, remove a method for aluminum chloride, the chlorosilane that contains aluminum chloride distilled, the volatile matter after distillation through be equipped with sylvite container reaction and cooling after obtain chlorine purification silane, specifically comprise 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 that contains aluminum chloride and sylvite is added to thermal distillation in the first distillation tower 2, distillation temperature is 65 DEG C, volatile matter is entered to the interior removal of impurities of the first trash separator 3, in the first trash separator 3, be filled with absorbent particles, 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 to keep the temperature in the first trash separator 36 be 180 DEG C, and the pressure of controlling in the first trash separator 3 is 0.2Mpa;
The volatile matter after step a the first trash separator 3 removal of impurities is entered surge tank 4 by b;
The chlorosilane that contains impurity in c surge tank (4) enters second column 5 and adds thermal distillation, distillation temperature is 180 DEG C, volatile matter is entered to the second trash separator 6, in the second trash separator 6, be filled with sylvite particle, the granularity of sylvite is 160 orders, porosity in the 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 to keep the temperature in the second trash separator 6 be 210 DEG C, and the pressure of controlling 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 condensations.
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 (10)
1. a method of removing aluminum chloride from chlorosilane, is characterized in that, the chlorosilane that contains aluminum chloride is distilled, the volatile matter after distillation through be equipped with sodium salt or sylvite container reaction and cooling after obtain chlorine purification silane.
2. a kind of method of removing aluminum chloride from chlorosilane according to claim 1, is characterized in that, specifically comprises the following steps:
A adds thermal distillation by the chlorosilane that contains aluminum chloride in the first distillation tower (2), and distillation temperature is 45-65 DEG C, and volatile matter is entered to the interior removal of impurities of the first trash separator (3), and the first trash separator is filled with sorbent material in (3);
The volatile matter after step a the first trash separator (3) removal of impurities is entered surge tank (4) by b;
The chlorosilane that contains impurity in c surge tank (4) enters second column (5) and adds thermal distillation, and distillation temperature is 180-195 DEG C, and volatile matter is entered to 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.
3. a kind of method of removing aluminum chloride from chlorosilane according to claim 2, 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%.
4. a kind of method of removing aluminum chloride from chlorosilane according to claim 2, 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.
5. a kind of method of removing aluminum chloride from chlorosilane according to claim 2, it is characterized in that, in the 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.
6. a kind of method of removing aluminum chloride from chlorosilane according to claim 2, is characterized in that, adds sodium salt or sylvite with aluminum chloride mass percent 90%-110% before step a distillation in the chlorosilane that is first containing aluminum chloride.
7. a kind of method of removing aluminum chloride from chlorosilane according to claim 2, 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 to keep the temperature in the second trash separator (6) be 180-210 DEG C.
8. a kind of method of removing aluminum chloride from chlorosilane according to claim 2, is characterized in that, the pressure in the first trash separator (3) and the second trash separator (6) is 0.15-0.2Mpa.
9. a kind of method of removing aluminum chloride from chlorosilane according to claim 2, it is characterized in that, sodium salt in 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.
10. the device of an a kind of method of removing aluminum chloride from chlorosilane claimed in claim 2, it is characterized in that, comprise successively former liquid storage tank (1), the first distillation tower (2), the first trash separator (3), surge tank (4), second column (5), the second trash separator (6), condenser (7) and purification storage tank (8), former liquid storage tank is connected with the first distillation tower (2) bottom, the first distillation tower (2) top is connected with the first trash separator (3), the 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 all connect by pipeline, front and the front strainer (11) that is also provided with of purification storage tank (8) at second column (5).
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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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