CN105396525B - A kind of closed pyroreaction kettle - Google Patents
A kind of closed pyroreaction kettle Download PDFInfo
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- CN105396525B CN105396525B CN201510728500.1A CN201510728500A CN105396525B CN 105396525 B CN105396525 B CN 105396525B CN 201510728500 A CN201510728500 A CN 201510728500A CN 105396525 B CN105396525 B CN 105396525B
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- autoclave body
- heat
- flange
- kettle
- kettle cover
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Abstract
The invention belongs to, and in particular to a kind of reaction kettle technical field, and in particular to closed high-temperature high-pressure reaction kettle；Including autoclave body (1), sealing ring (2), kettle cover (3) and retainer (4), the autoclave body (1) is the hollow cylinder tubular of one end open；The kettle cover (3) is the solid cylinder that one end is equipped with flange B (302)；The diameter of the kettle cover (3) is less than the internal diameter of autoclave body (1), and autoclave body (1) is placed on kettle cover (3) periphery；The sealing ring (2) is set to retainer (4), and retainer (4) is that circular ring shape is set between autoclave body (1) upper edge and the contact surface of flange (302) lower edge.
Description
Technical field
The invention belongs to reaction kettle technical fields, and in particular to a kind of closed high-temperature high-pressure reaction kettle.
Background technology
The present invention relates to a kind of closed pyroreaction kettles, determine in year synthesis benzene method before analysis sample in particular for 14C
Processing stage is the intermediate steps preparation Li2C2 for synthesizing benzene using the reaction kettle.It is anti-in 900 DEG C of high temperature by metal Li and CO2
1h is answered to synthesize Li2C2.During the reaction, CO2 in outside air must be avoided to be mixed into, it is desirable that reaction kettle has good seal
And Temperature Distribution.For ease of being put into metal Li and cleaning container, rubber sealing is used between kettle cover and autoclave body.And cushion rubber is in high temperature
Leakproofness drastically deteriorates in environment, needs to do heat-insulated, Cooling Design to the hermetic unit and reaction cavity segment of reaction kettle thus.Instead
It answers the reaction cavity segment of kettle to be placed directly in vertical crucible furnace to heat, temperature is higher when work, is equipped on reaction chamber top heat-insulated
Slot, heat dam top are equipped with spiral cooling water channel, and water channel top is sealing surface.By heat exchanger components, heat insulating member and reaction kettle collection
At obtaining that compact-sized, obturation effect is good, changes high-temperature closed reaction kettle easy to clean.
Existing reaction kettle is without heat dam, and the partial heat in reaction chamber conducts upwards along reaction kettle side wall, and thermal resistance is small, because
Thermal loss is larger when this such reaction kettle work.In addition, existing reaction kettle uses cooling water by being wrapped in reaction kettle top
Copper pipe to kettle body cool down, copper pipe and autoclave body lateral wall contact area are small, and heat exchange area is limited, such reaction kettle cooling efficiency compared with
Low, the temperature of sealing surface is excessively high, causes sealing ring aging very fast, and sealing cannot be guaranteed, thus is easy CO2 shadows in by air
Pilot causes dating precision to be deteriorated.
Compared with existing reaction kettle, reaction kettle sealed reliable, the service life in invention are long, save a large amount of cooling waters, earthenware
Crucible stove heat power lost is relatively low.While improving sample pre-treatments quality, energy expenditure is significantly saved.
Invention content
The purpose of the present invention, in view of the shortcomings of the prior art, it is to make synthesis Li to provide a kind of2C2Procedure seals are reliable, improve life
Object sample14C determines the closed pyroreaction kettle with heat dam and milling spiral cooling water channel of year precision.
The technical scheme is that：
A kind of closed pyroreaction kettle, including autoclave body, sealing ring, kettle cover and retainer, the autoclave body are one end open
Hollow cylinder tubular；Kettle cover position one end is equipped with the solid cylinder of flange B；The diameter of the kettle cover is less than the interior of autoclave body
Diameter, autoclave body are placed on kettle cover periphery；The sealing ring is set to retainer, and retainer is that circular ring shape is set to autoclave body upper edge and flange lower edge
Contact surface between.
The autoclave body includes reaction chamber, heat dam, return pipe, ring for the sealing liquid, spiral channel, water inlet pipe and flange A, wherein institute
The hollow cylinder tubular that autoclave body is one end open is stated, reaction chamber is its hollow cavity, and heat dam is equipped in the middle part of autoclave body outer wall, every
The autoclave body outer wall of heat channel upper end is equipped with spiral channel, and spiral channel the top water channel is equipped with through water pipe, on the water channel of bottom
Equipped with return pipe；Flange is set at autoclave body upper opening.
The kettle cover includes heat-insulation chamber, flange B, air inlet pipe, relief tube and escape pipe, and wherein flange B is set on heat-insulation chamber
Side, tracheae, relief tube and escape pipe pass through heat-insulation chamber.
The beneficial effects of the invention are as follows：
The mosaic structure heat dam of reaction kettle has the advantages that thermal resistance is high, intensity is high, along heat-insulated when reaction kettle being made to work
Temperature distribution gradients on slot vertical direction are larger.Thermal loss is few when with existing reaction kettle than work, and cooling load is small, accomplishes
Energy-saving and water-saving.
Milling spiral cooling water channel effectively increases autoclave body heat dissipation area, and more existing reaction kettle heat exchange efficiency is high, to protect
Demonstrate,prove the operating temperature that autoclave body flange temperature is no more than seal.
Kettle cover heat-insulation chamber outer ring surface and reaction kettle body gap very little, and the relatively thin thermal resistance of heat-insulated cavity outer wall is larger, ensures kettle
Lid flange temperature is no more than the operating temperature of seal.
Rubber sealing is used between kettle cover and autoclave body, convenient for being put into metal Li and cleaning container, and sealed reliable, is ensured
The accurate measurement of 14C.
Description of the drawings
Fig. 1 is reaction kettle overall structure diagram；
Fig. 2 is kettle structure figure；
Fig. 3 is kettle cover structure chart；
Fig. 4 is seal ring assembly schematic diagram.
Specific implementation mode
A kind of closed pyroreaction kettle proposed by the present invention is further introduced with embodiment below in conjunction with the accompanying drawings：
A kind of closed pyroreaction kettle, including autoclave body 1, sealing ring 2, kettle cover 3 and retainer 4, the autoclave body 1 are opened for one end
The hollow cylinder tubular of mouth；3 one end of the kettle cover are equipped with the solid cylinder of flange B302；The diameter of the kettle cover 3 is small
In the internal diameter of autoclave body 1, autoclave body 1 is placed on 3 periphery of kettle cover；The sealing ring 2 is set to retainer 4, and retainer 4 is that circular ring shape is set to kettle
Between the contact surface of 302 lower edge of 1 upper edge of body and flange.
The autoclave body 1 includes reaction chamber 101, heat dam 102, return pipe 103, ring for the sealing liquid 104, spiral channel 105, water inlet
Pipe 106 and flange A107, wherein the autoclave body 1 is the hollow cylinder tubular of one end open, reaction chamber 101 is in its is hollow
Chamber, 1 outer wall of autoclave body middle part are equipped with heat dam 102, and 1 outer wall of autoclave body of 102 upper end of heat dam is equipped with spiral channel 105, spiral
105 the top water channel of water channel is equipped with through water pipe 106, and bottom water channel is equipped with return pipe 103；Flange 1 is set to 1 top of autoclave body
Opening.
The kettle cover 3 includes heat-insulation chamber 301, flange B302, air inlet pipe 303, relief tube 304 and escape pipe 305, wherein method
Blue B302 is set to 301 upside of heat-insulation chamber, and tracheae 303, relief tube 304 and escape pipe 305 pass through heat-insulation chamber 301.
Embodiment 1
Metal Li is put into reaction kettle body bottom, and assembly relation consolidates autoclave body and kettle cover as shown in Figure 1.Close pressure release
Pipe and air inlet pipe are opened the effective vacuum pump of outlet and are vacuumized to reaction kettle.The water inlet pipe and return pipe of reaction kettle are opened, is connected cold
But water, and reactor bottom is packed into crucible furnace.It slowly heats, the petroleum ether on the surfaces metal Li is vaporized, with air in kettle one
With extraction.700 DEG C are heated to, air inlet pipe is opened, is slowly introducing the CO2 of purified processing.900 DEG C are warming up to, constant temperature 1h, CO2
The reaction was complete with metal Li, is then evacuated 15min.Electric furnace is closed, is cooled to room temperature.
During reacting progress, crucible furnace reacts cavity segment to reaction kettle by heat radiation and conduction and heats.Reaction kettle
A heat part for acquisition maintains the progress of reaction, another part to continue up conduction, reaction kettle heat dam along reaction kettle side wall
For similar mosaic structure, on the one hand improving thermal resistance keeps distribution gradient of the temperature on heat dam vertical direction larger, another party
Face ensures the higher structural strength of autoclave body.It is absorbed by spiral cooling water channel by the heat of heat dam, to ensure autoclave body flange
Upper surface temperature is in zone of reasonableness, it is ensured that sealed reliable.Inside reaction kettle, CO2 temperature is passed at 900 DEG C or so by heat
The mode led transfers heat to the heat-insulated cavity outer wall of kettle cover.Because of heat-insulation chamber outer ring surface and reaction kettle body gap very little, gap location
Gaseous exchange effect is poor, can ignore the heat transfer of outer ring surface.Relatively thin its thermal resistance thus of the heat-insulated cavity outer wall of kettle cover is larger, effectively
Ensure kettle cover flange undersurface temperature in zone of reasonableness, it is ensured that sealed reliable.
Spiral cooling water channel is the helicla flute gone out in autoclave body top Milling Process, to effectively increase the radiating surface of autoclave body
Product.And in its outer circle tight fit ring for the sealing liquid, it is ensured that cooling water not channelling between different circles.Ring for the sealing liquid inner wall is at upper and lower end face
Contact position corresponding to autoclave body sealing welding.Ring for the sealing liquid corresponding position sealing welding at spiral channel upper and lower side is connected to water inlet pipe and returns
Water pipe, for connecting cooling water system.
Claims (2)
1. a kind of closed pyroreaction kettle, it is characterised in that：Including autoclave body (1), sealing ring (2), kettle cover (3) and retainer (4),
The autoclave body (1) is the hollow cylinder tubular of one end open；The kettle cover (3) is the filled circles that one end is equipped with flange B (302)
Cylinder；The diameter of the kettle cover (3) is less than the internal diameter of autoclave body (1), and autoclave body (1) is placed on kettle cover (3) periphery；The sealing ring (2)
Set on retainer (4), retainer (4) is that circular ring shape is set between autoclave body (1) upper edge and the contact surface of flange B (302) lower edge；
The autoclave body (1) includes reaction chamber (101), heat dam (102), return pipe (103), ring for the sealing liquid (104), spiral channel
(105), water inlet pipe (106) and flange A (107), wherein the autoclave body (1) is the hollow cylinder tubular of one end open, reaction
Chamber (101) is its hollow cavity, is equipped with heat dam (102) in the middle part of autoclave body (1) outer wall, the autoclave body (1) of heat dam (102) upper end is outside
Wall is equipped with spiral channel (105), and spiral channel (105) the top water channel is equipped with through water pipe (106), is set on the water channel of bottom
There is return pipe (103)；Flange A (107) is set at autoclave body (1) upper opening.
2. a kind of closed pyroreaction kettle as described in claim 1, it is characterised in that：The kettle cover (3) includes heat-insulation chamber
(301), flange B (302), air inlet pipe (303), relief tube (304) and escape pipe (305), wherein flange B (302) are set to heat-insulated
On the upside of chamber (301), tracheae (303), relief tube (304) and escape pipe (305) pass through heat-insulation chamber (301).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510728500.1A CN105396525B (en) | 2015-10-30 | 2015-10-30 | A kind of closed pyroreaction kettle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510728500.1A CN105396525B (en) | 2015-10-30 | 2015-10-30 | A kind of closed pyroreaction kettle |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105396525A CN105396525A (en) | 2016-03-16 |
| CN105396525B true CN105396525B (en) | 2018-09-28 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510728500.1A Active CN105396525B (en) | 2015-10-30 | 2015-10-30 | A kind of closed pyroreaction kettle |
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| CN (1) | CN105396525B (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106861557B (en) * | 2017-04-24 | 2023-03-10 | 中国科学技术大学 | Volatilization device for CVD solid source |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100320135A1 (en) * | 2009-06-19 | 2010-12-23 | Wen-Chon Sun | Water purification kettle |
| CN203316120U (en) * | 2013-04-28 | 2013-12-04 | 贵研资源（易门）有限公司 | Heavy metal closed dissolution reaction kettle |
| CN103643199B (en) * | 2013-12-13 | 2016-02-24 | 东北大学 | A kind of Pressure nitrogenization furnace |
| CN205412960U (en) * | 2015-10-30 | 2016-08-03 | 核工业北京地质研究院 | Airtight pyroreaction cauldron |
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| CN105396525A (en) | 2016-03-16 |
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