CN202666872U - Molecular sieve regeneration equipment - Google Patents

Molecular sieve regeneration equipment Download PDF

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Publication number
CN202666872U
CN202666872U CN 201220346900 CN201220346900U CN202666872U CN 202666872 U CN202666872 U CN 202666872U CN 201220346900 CN201220346900 CN 201220346900 CN 201220346900 U CN201220346900 U CN 201220346900U CN 202666872 U CN202666872 U CN 202666872U
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CN
China
Prior art keywords
molecular sieve
adsorption tower
silane
nitrogen
regeneration
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Expired - Fee Related
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CN 201220346900
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Chinese (zh)
Inventor
桑艳青
耿金成
许宝辉
史东旭
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FINE SILICON Co Ltd
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FINE SILICON Co Ltd
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Priority to CN 201220346900 priority Critical patent/CN202666872U/en
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Abstract

The utility model discloses molecular sieve regeneration equipment, which comprises an adsorption tower (1), wherein the adsorption tower (1) is provided with a silicane inlet valve and a silicane outlet valve, and a molecular sieve is also arranged inside the adsorption tower (1); and the adsorption tower (1) is connected with a nitrogen conveying device for replacing silicane in the molecular sieve and performing desorption on impurities in the molecular sieve in the regeneration process of the molecular sieve. By the molecular sieve regeneration equipment, a regeneration process is simplified, hydrogen impurities are avoided, safety can be ensured, and the regeneration cost can also be reduced.

Description

Regenerating molecular sieve equipment
Technical field
The present invention relates to silane purification technology field, particularly a kind of regenerating molecular sieve equipment.
Background technology
Silane need to further be removed with molecular sieve through also containing the impurity of trace behind a series of rectifying devices, through obtaining electronic-grade silane after the molecular sieve adsorption removal of impurities.Adsorption function descends after molecular sieve adsorption impurity arrives to a certain degree, needs the molecular sieve regenerated offline this moment.
In the prior art, regenerating molecular sieve generally has two kinds of methods.The first, the patent No. is that " 201110255542.X ", patent name provide a kind of technique of utilizing product nitrogen gas to participate in molecular sieve adsorber regeneration for the patent of " a kind of technique of utilizing product nitrogen gas to participate in molecular sieve adsorber regeneration ", to go out between the product nitrogen gas pipeline of air separation and the dirty nitrogen pipeline and connect with pipeline, and install by-pass valve control additional, product nitrogen gas is introduced hot reactivation participate in molecular sieve adsorber regeneration with dirty nitrogen pipe, needn't too much eat the throttling air, can satisfy the demand of regenerating molecular sieve gas flow.More air are entered participate in rectifying in the tower, thereby can improve gas yield.But the technique that this kind renovation process and the present invention mention differs more, without comparativity.
The method of the second regeneration in the prior art, be exactly with nitrogen the silane in the molecular sieve to be replaced away first, then with hot hydrogen heating molecular sieve mode the impurity desorption of molecular sieve adsorption is gone out, heated gas flow is crossed molecular sieve, and the heating molecular sieve is also taken away the impurity in the microporous molecular sieve.
Method and the present invention of above-mentioned the second regenerating molecular sieve are nearer, but have following defective:
The first, molecular sieve silane displacement step just needs nitrogen, and regeneration need to switch to hydrogen, because the hydrogen molecule diameter is little, it is easy to enter in the aperture of molecular sieve, is easy to bring hydrogen impurity to silane purification technique.
The second, hydric safe is relatively poor.The hydrogen chemical property is active, and molecular volume is little, reveals easily, will form explosive mixture if reveal, and personnel and equipment are caused potential safety hazard.
The 3rd, the hydrogen cost is high.Also need to have improved the cost of regenerated molecular sieve with hydrogen regeneration with the complete rear usefulness of nitrogen replacement.
In view of this, how regenerating molecular sieve equipment in the prior art being made improvements, thereby simplify on the one hand regeneration technology and avoid bringing hydrogen impurity, can guarantee that on the other hand safety and health hangs down regeneration cost, is the problem that those skilled in the art need solution badly.
Summary of the invention
The technical problem to be solved in the present invention is for providing a kind of regenerating molecular sieve equipment, and this reclaim equiment design can be simplified on the one hand regeneration technology and avoid bringing hydrogen impurity, can guarantee that on the other hand safety and health hangs down regeneration cost.
For solving the problems of the technologies described above, the invention provides a kind of regenerating molecular sieve equipment, comprise adsorption tower, described adsorption tower is provided with silane imported valve and silane outlet valve, and the inside of described adsorption tower also is provided with molecular sieve; This adsorption tower is connected with for the nitrogen gas conveying device at the displacement of regenerating molecular sieve process silane and silane impurity desorption.
Preferably, also be provided with heater on the pipeline of described nitrogen gas conveying device.
Preferably, described heater is electric heater.
Preferably, described electric heater is provided with temperature controlling unit.
Preferably, also be connected with temperature indicator on the described adsorption tower.
Preferably, also be provided with the control valve of regulating nitrogen flow on the pipeline of described nitrogen gas conveying device.
In the present invention, the desorption of silane displacement and silane impurity all be suitable for nitrogen gas conveying device and finishes by supplying nitrogen, thereby has save the processing step of closing nitrogen valve and unlatching hydrogen valve in the prior art, thereby has simplified regeneration technology.In addition, when carrying out silane impurity desorption, or the nitrogen that adopts, thereby can avoid bringing again hydrogen impurity.Also have, in the present invention, nitrogen is inert gas, is not easy to and other material generation chemical reactions, can not burn and explode handling safety.At last, the cost of nitrogen is more much lower than hydrogen, thereby can save regeneration cost.
In sum, the design of regenerating molecular sieve equipment provided by the present invention can be simplified on the one hand regeneration technology and avoid bringing hydrogen impurity, can guarantee that on the other hand safety and health hangs down regeneration cost.
Description of drawings
Fig. 1 is the FB(flow block) of regenerating molecular sieve method in an embodiment of the present invention;
Fig. 2 is the structural representation of regenerating molecular sieve equipment in an embodiment of the present invention.
The specific embodiment
Core of the present invention is for providing a kind of regenerating molecular sieve method, and the design of this renovation process can be simplified on the one hand regeneration technology and avoid bringing hydrogen impurity, can guarantee that on the other hand safety and health hangs down regeneration cost.In addition, another core of the present invention is for providing a kind of regenerating molecular sieve equipment.
In order to make those skilled in the art understand better technical scheme of the present invention, the present invention is described in further detail below in conjunction with the drawings and specific embodiments.
At first, the used technical term of the present invention is made an explanation.
1, molecular sieve: the sorbing material of ethene in the absorption silane, type is the 4A molecular sieve;
2, adsorption tower: the equipment that is loaded with molecular sieve.
3, regeneration: behind the molecular sieve adsorption impurity ethene, utilize the hot gas mode of heating to remove the impurity of absorption in the molecular sieve (that is the silane impurity mentioned of the present invention, such as, above-mentioned ethene), reach a kind of method of molecular sieve recycling.
Please refer to Fig. 1 and Fig. 2, Fig. 1 is the FB(flow block) of regenerating molecular sieve method in an embodiment of the present invention; Fig. 2 is the structural representation of regenerating molecular sieve equipment in an embodiment of the present invention.
As shown in Figure 2, in the present invention, regenerating molecular sieve equipment comprises adsorption tower 1, and adsorption tower 1 is provided with silane imported valve and silane outlet valve, and the inside of adsorption tower 1 also is provided with molecular sieve; This adsorption tower 1 is connected with for the nitrogen gas conveying device at the displacement of regenerating molecular sieve process silane and silane impurity desorption.In addition, also be provided with heater 2 on the pipeline of nitrogen gas conveying device, this heater 2 is specially electric heater.
As shown in Figure 1, regenerating molecular sieve method provided by the present invention comprises the steps:
S 1: silane imported valve and the silane outlet valve of closing adsorption tower 1; Particularly, so that adsorption tower 1 leaves production line, and close silane imported valve and the silane outlet valve of adsorption tower 1.
S2: the silane in the adsorption tower 1 is cemented out with nitrogen; In adsorption tower 1, be filled with nitrogen by above-mentioned nitrogen gas conveying device, then be discharged into normal pressure, again be filled with nitrogen to adsorption tower 1, be discharged into normal pressure.So repeatedly, finish adsorption tower 1 pressurising pressure release displacement.
S3: keep nitrogen to carry, heater 2, the nitrogen by heating is with the silane impurity desorption on the adsorption tower 1 interior molecular sieve out.
In the present invention, the absorption of silane displacement and silane impurity be suitable for all that nitrogen finishes, thereby has save the processing step of closing nitrogen valve and unlatching hydrogen valve in the prior art, thereby has simplified regeneration technology.In addition, when carrying out silane impurity desorption, or the nitrogen that adopts, thereby can avoid bringing again hydrogen impurity.Also have, in the present invention, nitrogen is inert gas, is not easy to and other material generation chemical reactions, can not burn and explode handling safety.At last, the cost of nitrogen is more much lower than hydrogen, thereby can save regeneration cost.
To sum up, the design of regenerating molecular sieve method provided by the present invention can be simplified on the one hand regeneration technology and avoid bringing hydrogen impurity, can guarantee that on the other hand safety and health hangs down regeneration cost.
Particularly, can make specific design to above-mentioned renovation process.Such as, in above-mentioned steps S1, close the silane imported valve and outlet valve of adsorption tower 1 after, also need the earth pressure release in the adsorption tower 1 to normal pressure.
In addition, in above-mentioned steps S2, the mode by the pressurising pressure release cements out the silane in the adsorption tower 1 with nitrogen.Particularly, in adsorption tower 1, be filled with the nitrogen with larger pressure, and so that nitrogen fully mixes with silane, and then carry out pressure release, also can discharge silane when nitrogen discharges.
Particularly, in step S3, by the heating of heater 2, thereby so that 30 ° of temperature in the adsorption tower 1 are heated to 450 °.And further, heating process adopts the mode of notch cuttype heating.
Particularly, the heater 2 that is specially of the mode of notch cuttype heating improves heating-up temperature gradually, middlely changes a heating-up temperature every 30 ° ~ 50 °, until after the head temperature of adsorption tower 1 reaches this heating-up temperature, so that adsorption tower 1 insulation one hour.The design of this kind method can prevent that on the one hand the rapid rising of temperature from causing damage to molecular sieve, on the other hand can be so that the abundant desorption silane of hot nitrogen molecule impurity.
Further, until heating-up temperature reaches 450 °, and after the temperature at the top of tower upon adsorption 1 reaches 450 °, so that adsorption tower 1 insulation 8 ~ 10 hours.This kind structural design can be so that the hot nitrogen molecule fully adsorbs silane impurity.
As shown in Figure 1, can also make further design.Such as, also comprise the steps: after the above-mentioned steps S3
S4: turn down the temperature of heater 2, slowly make the temperature of adsorption tower 1 be reduced to 30 °.
The design of this kind method can prevent the rapid decline of temperature and cause molecular sieve is caused damage.
In addition, as shown in Figure 2, can also make specific design to regenerating molecular sieve equipment of the present invention.
Such as, electric heater is provided with temperature controlling unit, and this temperature controlling unit is convenient to the heating-up temperature of electric heater is controlled to adjust, thereby can be convenient to realize above-mentioned stairstepping mode of heating.
In addition, as shown in Figure 2, also be connected with temperature indicator 3 on the adsorption tower 1.This temperature indicator 3 is used for showing the temperature of adsorption tower 1, thereby is convenient to realize the control to temperature.
Moreover, as shown in Figure 2, also be provided with the control valve of regulating nitrogen flow on the pipeline of nitrogen gas conveying device.Regulate the flow of nitrogen by this control valve, thereby can according to what of impurity on the molecular sieve, correspondingly regulate the flow of nitrogen.
More than regenerating molecular sieve method provided by the present invention and reclaim equiment are described in detail.Used specific case herein principle of the present invention and embodiment are set forth, the explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof.Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of claim of the present invention.

Claims (6)

1. a regenerating molecular sieve equipment comprises adsorption tower (1), and described adsorption tower (1) is provided with silane imported valve and silane outlet valve, and the inside of described adsorption tower (1) also is provided with molecular sieve; It is characterized in that this adsorption tower (1) is connected with for the nitrogen gas conveying device at the displacement of regenerating molecular sieve process silane and silane impurity desorption.
2. regenerating molecular sieve equipment as claimed in claim 1 is characterized in that, also is provided with heater (2) on the pipeline of described nitrogen gas conveying device.
3. regenerating molecular sieve equipment as claimed in claim 2 is characterized in that, described heater (2) is electric heater.
4. regenerating molecular sieve equipment as claimed in claim 3 is characterized in that, described electric heater is provided with temperature controlling unit.
5. regenerating molecular sieve equipment as claimed in claim 1 is characterized in that, also is connected with temperature indicator (3) on the described adsorption tower (1).
6. such as each described regenerating molecular sieve equipment of claim 1 to 5, it is characterized in that, also be provided with the control valve of regulating nitrogen flow on the pipeline of described nitrogen gas conveying device.
CN 201220346900 2012-07-17 2012-07-17 Molecular sieve regeneration equipment Expired - Fee Related CN202666872U (en)

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Application Number Priority Date Filing Date Title
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102716731A (en) * 2012-07-17 2012-10-10 六九硅业有限公司 Molecular sieve regeneration method and equipment
CN104324688A (en) * 2014-10-21 2015-02-04 杭州中泰深冷技术股份有限公司 System and method for regenerating molecular sieve and saving energy by using low-pressure nitrogen
CN104548871A (en) * 2015-01-19 2015-04-29 河南心连心化肥有限公司 High-efficiency molecular sieve regeneration device and process thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102716731A (en) * 2012-07-17 2012-10-10 六九硅业有限公司 Molecular sieve regeneration method and equipment
CN104324688A (en) * 2014-10-21 2015-02-04 杭州中泰深冷技术股份有限公司 System and method for regenerating molecular sieve and saving energy by using low-pressure nitrogen
CN104324688B (en) * 2014-10-21 2016-09-14 杭州中泰深冷技术股份有限公司 One low-pressure nitrogen carries out regenerating molecular sieve energy conserving system and method
CN104548871A (en) * 2015-01-19 2015-04-29 河南心连心化肥有限公司 High-efficiency molecular sieve regeneration device and process thereof
CN104548871B (en) * 2015-01-19 2016-10-19 河南心连心化肥有限公司 Molecular sieve high-efficient regenerating unit and technique thereof

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CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20130116

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CF01 Termination of patent right due to non-payment of annual fee