CN207209961U

CN207209961U - A kind of energy-efficient high purity silicon nitride manganese production system

Info

Publication number: CN207209961U
Application number: CN201720681308.6U
Authority: CN
Inventors: 王兆兵; 姚发艳
Original assignee: Individual
Current assignee: Individual
Priority date: 2017-06-13
Filing date: 2017-06-13
Publication date: 2018-04-10
Anticipated expiration: 2027-06-13

Abstract

The utility model discloses a kind of energy-efficient high purity silicon nitride manganese production system, mainly including electric furnace（19）, retort（1）, cooler（2）, rough vacuum pump（16）, rich nitrogen basin（13）, hydrogenation purifier（12）, pure nitrogen gas basin（10）, reduction gas-reservoir tank（5）, blender（8）, it is characterised in that：The electric furnace（19）Inside it is provided with branched retort（1）, the retort（1）With cooler（2）, pump intake valve（17）, rough vacuum pump（16）, pump out air valve（14）, rich nitrogen basin（13）, hydrogenation purifier（12）, booster fan（11）, pure nitrogen gas basin（10）, rush nitrogen valve（9）It is sequentially connected by pipeline, forms the atmosphere displacement loop of system, while for nitrogenizing.Life cycle of the product of the present utility model is short, and production cost is low, less energy consumption, and nitrogen utilization rate is high, and product purity is high.

Description

A kind of energy-efficient high purity silicon nitride manganese production system

Technical field

It the utility model is related to the production field of additive nitrogenized manganese in Ferrous Metallurgy, and in particular to high purity silicon nitride manganese Production technology.

Background technology

The development of special steel increases the demand of nitrogenized manganese, particularly high to nitrogen and manganese element content, other impurities element The low high-quality nitrogenized manganese demand of content is more.

The production method of many nitrogenized manganeses is currently suggested, used nitridation equipment has tube furnace, fluidized-bed reaction Stove, rotary furnace etc.；Pressurization（Nitridation pressure is more than 0.1 MPa）, it is used nitridation equipment have vacuum resistance furnace, shaft furnace, Nitriding furnace etc., and realize that the related device of scale metaplasia is (the track type vacuum nitride resistive of the patent No. 200910044526.9 Stove), the yield of annual nitrogenized manganese has more than ten thousand tons, obtains preferable economic benefit, but there is also following shortcoming：

（1）Process units power consumption is higher, 10Pa condition of high vacuum degree before technological requirement nitridation reaction, has used two class large powers Vacuum pump assembly, and nitrogenize material and only account for the 15~20% of furnace volume, relative nullity space is also big so that the pumpdown time Up to 10~12 hours, take and consume energy again, while in order to prevent furnace shell temperature distortion, be provided with stove outer covering water spray system, band Amount of heat is walked, device 750 DEG C of power consumption of product synthesis per ton early stage, for later stage device by improving, comprehensive power consumption also there are 500 DEG C.

（2）Whole device fixed investment is high, is up to 40~48 hours per the stove production cycle.Pure nitrogen gas utilization rate is low, scale It is lost in metaplasia production big.

（3）Mn oxide content is high in product, and device could not reduce to manganese oxide；Directly heat, heating electrode is Carbon electrode, carbon material can volatilize effusion, penetrate into product, polluted product, make product carbon easily exceeded.

Also there is technical scheme to propose to rush the nitrogenous reducibility gas such as ammonia or ammonia pyrolysis gas into stove, reaction production water could not and When discharge, vapor partial pressure is high, is unfavorable for continuing for reduction reaction, most manganese oxide could not restore.

The content of the invention

The utility model aims to overcome that insufficient existing for above-mentioned technology, there is provided a kind of energy-efficient high purity silicon nitride Manganese production system, the system remove the oxygen reduction in raw material, improve the quality of product, reduce the time consumption and energy consumption in production.

The technical solution of the utility model is as follows：A kind of energy-efficient high purity silicon nitride manganese production system, it is main to include electricity It is heating furnace, retort, cooler, rough vacuum pump, rich nitrogen basin, hydrogenation purifier, reduction gas-reservoir tank, pure nitrogen gas basin, mixed Clutch, is provided with branched retort in the electric furnace, the retort and cooler, pump intake valve, rough vacuum pump, pumps out Air valve, rich nitrogen basin, hydrogenation purifier, booster fan, pure nitrogen gas basin, rush nitrogen valve and be sequentially connected by pipeline, form system The atmosphere displacement loop of system, while for nitrogenizing；The retort and cooler, reduction air outlet valve, clarifier, reduction gas-reservoir Tank, booster fan, blender, reduction intake valve are sequentially connected by pipeline, form the reduction loop of system.

Further, on the atmosphere displacement loop of system, the rough vacuum pump outlet conduit is provided with exhaust-valve, described cold But device outlet be provided with moisture detector and oxygen, hydrogen detector and safe draining valve, the pure nitrogen gas basin by pipeline with Nitrogen making machine is connected, for supplementing displacement nitrogen source and nitridation nitrogen source.

Further, on the reduction loop of system, the blender has branched pipe to be connected with ammonia cracker, for supplementing also Protohydrogen gas, the blender separately have branched pipe to be connected with hydrogenation purifier, and the hydrogenation for rich nitrogen purifies.

Further, the retort is placed in electricity plus stove, and outside stove, electric furnace is provided with automatic constant at retort both ends Warm heater, electric furnace bottom are provided with nitrogenized manganese cooling tank car；

Further, upper and lower end has thermal radiation resistant division board in the retort, and the material of retort is high temperature resistance and high strength Steel alloy, 300~420mm of diameter of retort, 2000~4000mm of length, 30~60mm of wall thickness, is obtained by centrifugal casting.

The beneficial effects of the utility model are.

1st, retort has that volume is big, can account for total measurement (volume) 80%, and the production cycle of product shortens, and passes through atmosphere in retort Oxygen content in retort, can just be down to 0.5% for 2 hours, the production cycle of a batch products can be controlled in 12 hours by displacement It is interior.

2nd, production cost is low, and energy consumption is reduced, and nitrogen utilization rate is high, and product power consumption per ton is down to 400 degree of electricity.

3rd, product purity is high, and host element nitrogen, manganese and value are up to more than 99%.

Brief description of the drawings：

Fig. 1 is production system connection figure of the present utility model.

Embodiment：

1 illustrate the technical solution of the utility model, a kind of energy-efficient high purity silicon nitride manganese below in conjunction with the accompanying drawings Production system, mainly include electric furnace 19, retort 1, cooler 2, rough vacuum pump 16, rich nitrogen basin 13, hydrogenation purifying Device 12, pure nitrogen gas basin 10, gas-reservoir tank 5, blender 8 are reduced, branched retort 1 is provided with the electric furnace 19, it is described Retort 1 and cooler 2, pump intake valve 17, rough vacuum pump 16, pump out air valve 14, rich nitrogen basin 13, hydrogenation purifier 12, Booster fan 11, pure nitrogen gas basin 10, rush nitrogen valve 9 and be sequentially connected by pipeline, form the atmosphere displacement loop of system, use simultaneously In nitridation；The retort 1 and cooler 2, reduction air outlet valve 3, clarifier 4, reduction gas-reservoir tank 5, booster fan 6, blender 8th, reduction intake valve 7 is sequentially connected by pipeline, forms the reduction loop of system.

Further, on the atmosphere displacement loop of system, the outlet conduit of rough vacuum pump 16 is provided with exhaust-valve 15, institute Cooler outlet pipe is stated provided with moisture detector 20 and oxygen, hydrogen detector 22 and safe draining valve 21, the pure nitrogen gas basin 10 are connected by pipeline with nitrogen making machine 24, for supplementing displacement nitrogen source and nitridation nitrogen source.

Further, on the reduction loop of system, the blender 8 has branched pipe to be connected with ammonia cracker 23, for also Former hydrogen make-up, the blender 8 separately have branched pipe to be connected with hydrogenation purifier 12, and the hydrogenation for rich nitrogen purifies.

Further, the retort 1 is placed in electricity plus stove 19, and the both ends of retort 1 are outside electricity plus stove 19, electric furnace 19 Automatic constant temperature heating device 18 is provided with, electric furnace bottom is provided with nitrogenized manganese cooling tank car 25.

Further, upper and lower end has thermal radiation resistant division board 26 in the retort 1, and the material of retort 1 is high temperature resistant height Strength alloys steel, is obtained by centrifugal casting, 300~420mm of diameter of retort, 2000~4000mm of length, and wall thickness 30~ 60mm。

Specific work process of the present utility model is as follows：

The first step, feed sealed cans, the raw materials such as electrolytic manganese metal piece or manganese powder is loaded in retort 1, sealed shell of tank.

Second step, atmosphere displacement：

(a) exhaust is once evacuated：Gas in retort 1 is quickly taken out with rough vacuum pump 16, gas bleeding emptying, is evacuated to absolute pressure After 0.05MPa, stop pumping, pure nitrogen gas in pure nitrogen gas basin 10 is poured into retort 1, after pressure reaches 0.2MPa, stop Nitrogen is rushed, gas in retort 1 is discharged to rich nitrogen basin 13.

(b) it is secondary to evacuate recovery：Continued the gas of retort 1 being extracted into rich nitrogen basin 13 with rough vacuum pump 16, be evacuated to After the MPa of absolute pressure 0.05, pure nitrogen gas is rushed into retort 1 again, stops rushing nitrogen after 0.2 MPa of pressure, by retort 1 Gas is discharged to rich nitrogen basin 13.

(c) recovery is evacuated three times：The b that repeats the above steps is operated, when oxygen, hydrogen detector 22 check that the oxygen content in exhaust is low In less than 0.5%, displacement is completed.

(d) it is hydrogenated with purification：It is recovered to the hydrogen that the rich nitrogen ammonia cracker 23 of rich nitrogen basin 13 cracks out Body carries out hydrogenation purifying, it is purified, generate water except dereaction after, obtain pure nitrogen gas, store reuse.

3rd step, start to start electric heater unit 18 when carrying out second step.

4th step, when in-furnace temperature is raised to 800 DEG C.

（a）The also Primordial Qi that blender 8 has matched is passed through retort 1, wherein hydrogen content 30~50%, and surplus is nitrogen, dimension The MPa of pressure 0.05,850~950 DEG C of temperature are held, discharge gas hydrogen content maintains continuous 10~30%, and discharge gas cools down only through cooler 4 Change, be recovered to reduction gas-reservoir tank 5, and exhaust moisture is detected with moisture detector 20.

（b）When exhaust moisture is less than 0.1g/Nm³When, illustrate that the combination oxygen more than 90% in manganese oxide is reduced, change Pure nitrogen gas is passed through, discharge air cooling, purifies, be recovered to reduction gas-reservoir tank 5, when oxygen, the detection exhaust hydrogen content of hydrogen detector 22 are small Stop discharge gas when 2%.

5th step, nitridation continue to rush pure nitrogen gas, the MPa of pressure 0.2 in maintenance reaction tank 1,950~1050 DEG C of temperature, 4~ 6 hours, it is ensured that higher nitrogen partial pressure, Accelerate nitriding reaction, lift nitrogen content in manganese.

6th step, pressurize cooling, keeps the MPa of pressure 0.2, stops heating, cooling.

7th step, nitrogen protection cooling, when temperature drops to 500 DEG C pressure release open flange, discharging to cooling tank to normal pressure Car 25, nitrogen is rushed into tank, product is cooled to less than 200 DEG C under nitrogen protection.

Claims

A kind of 1. energy-efficient high purity silicon nitride manganese production system, mainly including electric furnace（19）, retort（1）, cooler （2）, rough vacuum pump（16）, rich nitrogen basin（13）, hydrogenation purifier（12）, pure nitrogen gas basin（10）, reduction gas-reservoir tank（5）、 Blender（8）, it is characterised in that：The electric furnace（19）Inside it is provided with branched retort（1）, the retort（1）With it is cold But device（2）, pump intake valve（17）, rough vacuum pump（16）, pump out air valve（14）, rich nitrogen basin（13）, hydrogenation purifier（12）、 Booster fan（11）, pure nitrogen gas basin（10）, rush nitrogen valve（9）It is sequentially connected by pipeline, forms the atmosphere displacement loop of system, Simultaneously for nitrogenizing；The retort（1）With cooler（2）, reduction air outlet valve（3）, clarifier（4）, reduction gas-reservoir tank（5）、 Booster fan（6）, blender（8）, reduction intake valve（7）It is sequentially connected by pipeline, forms the reduction loop of system；

The rough vacuum pump（16）Outlet conduit is provided with exhaust-valve（15）, the cooler outlet pipe is provided with moisture detector （20）With oxygen, hydrogen detector（22）With safe draining valve（21）, the pure nitrogen gas basin（10）Pass through pipeline and nitrogen making machine（24） It is connected；

The blender（8）Have branched pipe respectively with ammonia cracker（23）With hydrogenation purifier（12）It is connected.
A kind of 2. energy-efficient high purity silicon nitride manganese production system according to claim 1, it is characterised in that the reaction Tank（1）It is placed on electricity plus stove（19）It is interior, retort（1）Both ends are in electricity plus stove（19）Outside, electric furnace（19）It is provided with automatic constant Warm heater（18）, electric furnace bottom is provided with nitrogenized manganese cooling tank car（25）.
3. a kind of energy-efficient high purity silicon nitride manganese production system according to claim 1 or 2, it is characterised in that described Retort（1）Interior upper and lower end has thermal radiation resistant division board（26）, retort（1）Material be high temperature resistance and high strength alloy steel, lead to Cross centrifugal casting to obtain, 300~420mm of diameter of retort, 2000~4000mm of length, 30~60mm of wall thickness.