CN203990659U - A kind of easy device system of preparing loaded catalyst - Google Patents

A kind of easy device system of preparing loaded catalyst Download PDF

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Publication number
CN203990659U
CN203990659U CN201420155743.1U CN201420155743U CN203990659U CN 203990659 U CN203990659 U CN 203990659U CN 201420155743 U CN201420155743 U CN 201420155743U CN 203990659 U CN203990659 U CN 203990659U
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China
Prior art keywords
tower
stainless
steel
gas
wire box
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Expired - Fee Related
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CN201420155743.1U
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Chinese (zh)
Inventor
侯兴明
郭丹
石斌
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China University of Petroleum East China
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China University of Petroleum East China
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Priority to CN201420155743.1U priority Critical patent/CN203990659U/en
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Abstract

Prepare an easy device system for loaded catalyst, especially prepare the device system of loaded catalyst by vapor phase method.Device is made up of gas bomb, gas control valve, spinner flowmeter, seal head, tubular heater, porcelain boat, stainless (steel) wire box, cooling surge tank, solid paraffin tower, NaOH tower, calcium chloride tower.Raw material is high-temperature gasification in heating tube, to the carrier gas that passes into certain flow in tubular heater, the catalyst carrier of feed stream in stainless (steel) wire box that gasification produces carried in carrier gas, raw material is loaded in catalyst carrier, unreacted raw material is through the recycling use of supercooling surge tank, not recoverablely progressively processes completely through solid paraffin tower, NaOH tower, calcium chloride tower.It has overcome conventional tubular heating furnace preparing that in loaded catalyst process, load is inhomogeneous, sealing is poor, unreacting gas can not be recycled again and the shortcoming such as tail gas pollution environment, has produced certain economy and environment protecting.

Description

A kind of easy device system of preparing loaded catalyst
Technical field
The utility model relates to equipment technical field prepared by catalyst, is specifically related to one and prepares gas phase supported catalyst equipment.
Background technology
At present, when vapor phase method is prepared loaded catalyst, there is poor sealing in tubular heater conventionally, and the load factor of carrier is not high, and tail gas can not rationally be processed and recycle, and caused waste and the environmental pollution of raw material.
Summary of the invention
The subject matter that the utility model solves is the shortcoming for background technology, a kind of good airproof performance is provided, catalyst raw material utilization rate is high, the loaded catalyst Preparation equipment that carrier loaded rate is high, adopt condensate buffering tank to recycle and reuse reacting superfluous raw material, not recoverable tail gas is absorbed and reduces environmental pollution.
The utility model solves the technical scheme that its technical problem adopts: a kind of preparation facilities system of loaded catalyst, comprises gas bomb, gas control valve, spinner flowmeter, seal head, tubular heater, porcelain boat, stainless (steel) wire box, cooling surge tank, solid paraffin tower, NaOH tower, calcium chloride tower etc.It is characterized in that, in the gas inlet pipe formula heating furnace of certain flow, carry in magnetic boat feed stream that gasification the produces catalyst carrier in stainless (steel) wire box, it is loaded in catalyst carrier, unreacted raw material is through the recycling use of supercooling surge tank, not recoverablely progressively processes completely through solid paraffin tower, NaOH tower, calcium chloride tower.
Described gas bomb, gas control valve, spinner flowmeter are connected successively by gas stainless-steel pipe, and described seal head is connected with the quartz ampoule of tubular heater by sealing ring; Described tubular heater is connected with cooling surge tank with spinner flowmeter respectively by seal head; Described cooling surge tank is connected successively with solid paraffin tower, NaOH tower, calcium chloride tower.In described tubular heater, be placed with porcelain boat, stainless (steel) wire box.
The heating tube of described tubular heater is quartz ampoule or carborundum tube, and tubular heater seal head is cut with the groove that the degree of depth is 0.1mm-5mm; Sealing ring is enclosed within the groove of seal head, and sealing ring thickness is 1-4mm, sealing ring resistance to compression 5-10MPa; In heating tube, being placed with stainless (steel) wire box diameter is 5mm-100mm; The stainless (steel) wire aperture using for 0.1-300 μ m, the stainless (steel) wire box number of plies be 1-8 layer, carrier is fixed in stainless (steel) wire box.
Described surge tank is double-layer stainless steel structure, in the middle of ectonexine stainless steel, is hollow, in the middle of two-layer stainless steel, is connected with recirculated cooling water, and ectonexine stainless steel spacing is 2-25mm.
Described catalyst is prepared system can be divided into three parts: the gas handling system 1) being made up of gas bomb, gas control valve, spinner flowmeter etc.; 2) the catalyst preparation system being formed by seal head, tubular heater, porcelain boat, stainless (steel) wire box etc.; 3) exhaust treatment system being formed by cooling surge tank, solid paraffin tower, NaOH tower, calcium chloride tower etc.
In the utility model one detailed description of the invention, gas flow is in spinner flowmeter enters official heating furnace, in pipe, carrying gas-phase activity component reacts with catalyst carrier, make the uniform active constituent of catalyst surface load last layer, unreacted gas-phase activity component reclaims the complete gas of unreacted by cooling surge tank together with gas, then remains a small amount of gaseous component and absorbs respectively by follow-up solid paraffin tower, NaOH tower, calcium chloride tower materials such as removing organic principle, acid, moisture successively.Wherein, control gas and enter speed and the flow of tubular heater by controlling spinner flowmeter, and the flow of gas has determined the size of condensate buffering tank, solid paraffin tower, NaOH tower, calcium chloride tower, has more determined the length in reaction time and the uniformity of catalyst surface active component.Load the catalyst carrier of active constituent can directly in described tubular heater, complete roasting, directly obtain the catalyst of activation.
If, not containing acidic materials, described exhaust treatment system can omit NaOH tower in the utility model.Therefore, will be understood by those skilled in the art that for described exhaust treatment system and can build rational equipment according to concrete needs.
The utility model has overcome conventional tubular heating furnace preparing that in loaded catalyst process, catalyst cupport is inhomogeneous, system sealing is poor, unreacting gas can not be recycled again and the shortcoming such as tail gas pollution environment, has produced certain economy and environment protecting.
Therefore the easy device system that prepared by loaded catalyst described in the utility model has important actual application value, can be applied to industrial production.
Below in connection with accompanying drawing and detailed description of the invention, the utility model is described in detail, but those skilled in the art are to be understood that, those skilled in the art, according to the technological know-how that discloses and itself have of the present utility model, can change or revise the utility model.Therefore, scope of the present utility model is not limited to following embodiment, and should only be limited by claims.
Brief description of the drawings
Accompanying drawing is catalyst preparation facilities system flow schematic diagram of the present utility model.
In figure, gas bomb 1, gas control valve 2, rotor flow 3, sealing ring 4, seal head 5, porcelain boat 6, stainless (steel) wire box 7, quartz ampoule 8, tubular heater 9, cooling surge tank, 10, solid paraffin tower 11, NaOH tower 12, calcium chloride tower 13 forms.
Detailed description of the invention
1, gas phase load method is prepared Ni/ γ-Al 20 3catalyst
With γ-Al 20 3for carrier, nickel is that to prepare Supported Nickel Catalyst be the method for commonly using to active component gas phase load method.Concrete grammar is for weighing 10g γ-Al 20 3be positioned in stainless (steel) wire box 6 and compress, stainless (steel) wire box 6 is put into quartz ampoule 8 middle parts, pass into N 2be warmed up to 200 DEG C, the dry carrier of processing, weighs the pure nitric acid acetone of 3g nickel and is put in porcelain boat 6, regulates carrier gas flux 20ml/min by spinner flowmeter 3, and preparation time 5h, then uses N 2at 150 DEG C, purge 2h, pass into hydrogen reducing, regulate carrier gas flux 20ml/min by spinner flowmeter 3, preparation time 2h, then uses N 2at 150 DEG C, purge 2h and obtain Ni/ γ-Al 20 3catalyst, reaction finishes to reclaim the nitric acid acetone nickel in condensate buffering tank 10.
2, chemical vapour deposition technique is prepared Ti/HMS catalyst
Detailed process is as follows: 5g HMS (30~60 order) is put into the stainless (steel) wire 7 of tubular heater quartz ampoule 8, compacting, puts into quartz ampoule 8 middle parts by stainless (steel) wire box 7, passes into N 2be warmed up to 400 DEG C, dry pretreatment 2.5h.By TiCl 4put into porcelain boat 6, put into quartz ampoule 8, use N 2carry saturated TiCl 4steam carries titanium processing, and the processing time is (0.5~6h), then uses N 2at 150 DEG C, purge 4h, obtain Ti/HMS catalyst, reaction finishes to reclaim TiCl in condensate buffering tank 10 4.
3, silica vapor phase method modification
Detailed process is as follows: 5g silica (60 order) is put into the stainless (steel) wire box 7 of tubular heater quartz ampoule 8, compacting, regulates carrier gas flux 50ml/min by spinner flowmeter 3, passes into N 2be warmed up to 200 DEG C, dry pretreatment 2.5h, puts into porcelain boat 6 by kh-570, uses N 2carry kh-570 steam and carry out surface modification treatment, the processing time is (2~3h), then uses N 2at 150 DEG C, purge 4h and remove unreacted kh-570, obtain the SiO 2 catalyst of surface modification, reaction finishes to reclaim the kh-570 in condensate buffering tank 10.

Claims (5)

1. prepare the easy device system of loaded catalyst for one kind, by gas bomb, gas control valve, spinner flowmeter, seal head, tubular heater, stainless (steel) wire box, cooling surge tank, solid paraffin tower, NaOH tower, calcium chloride tower forms, it is characterized in that, in the gas inlet pipe formula heating furnace of certain flow, carry in magnetic boat feed stream that gasification the produces catalyst carrier in stainless (steel) wire box, raw material is loaded in catalyst carrier, unreacted raw material is through the recycling use of supercooling surge tank, not recoverable through solid paraffin tower, NaOH tower, calcium chloride tower is progressively processed completely.
2. easy device system as claimed in claim 1, is characterized in that: tubular heater seal head is cut with groove, the degree of depth is 0.1mm-5mm.
3. easy device system as claimed in claim 1, is characterized in that: sealing ring is enclosed within the groove of seal head, and sealing ring thickness is 1-4mm, sealing ring resistance to compression 5-10MPa.
4. easy device system as claimed in claim 1, is characterized in that: in heating tube, be placed with stainless (steel) wire box, stainless (steel) wire box diameter is 5mm-100mm; The stainless (steel) wire aperture using for 0.1-300 μ m, the stainless (steel) wire box number of plies be 1-8 layer, carrier is fixed in stainless (steel) wire box.
5. easy device system as claimed in claim 1, is characterized in that: described surge tank is double-layer stainless steel structure, in the middle of ectonexine stainless steel, is hollow, in the middle of two-layer stainless steel, is connected with recirculated cooling water, and ectonexine stainless steel spacing is 2-25mm.
CN201420155743.1U 2014-04-02 2014-04-02 A kind of easy device system of preparing loaded catalyst Expired - Fee Related CN203990659U (en)

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Application Number Priority Date Filing Date Title
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110252272A (en) * 2019-06-17 2019-09-20 万华化学集团股份有限公司 A kind of method and device of continuous large scale preparation olefin epoxidation catalysts
CN112044474A (en) * 2020-09-13 2020-12-08 昆明理工大学 Device for preparing catalyst by in-situ impregnation in different gas atmospheres and using method

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110252272A (en) * 2019-06-17 2019-09-20 万华化学集团股份有限公司 A kind of method and device of continuous large scale preparation olefin epoxidation catalysts
CN110252272B (en) * 2019-06-17 2022-04-22 万华化学集团股份有限公司 Method and device for continuously preparing olefin epoxidation catalyst on large scale
CN112044474A (en) * 2020-09-13 2020-12-08 昆明理工大学 Device for preparing catalyst by in-situ impregnation in different gas atmospheres and using method

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

Granted publication date: 20141210

Termination date: 20150402

EXPY Termination of patent right or utility model