CN107140611B - A kind of novel high purity silicon nitride manganese process units - Google Patents
A kind of novel high purity silicon nitride manganese process units Download PDFInfo
- Publication number
- CN107140611B CN107140611B CN201710439129.6A CN201710439129A CN107140611B CN 107140611 B CN107140611 B CN 107140611B CN 201710439129 A CN201710439129 A CN 201710439129A CN 107140611 B CN107140611 B CN 107140611B
- Authority
- CN
- China
- Prior art keywords
- tank
- reactor tank
- valve
- reduction
- gas
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0637—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with metals not specified in groups C01B21/0607 - C01B21/0635, other than aluminium, titanium, zirconium or hafnium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a kind of novel high purity silicon nitride manganese process units, it mainly include regenerative gas heating furnace 21, reactor tank 1, cooler 2, rough vacuum pump 19 plus hydrogen purifier 14, the reactor tank 1 and cooler 2, pump intake valve 22, rough vacuum pump 19 pump out air valve 17, rich nitrogen basin 16 plus hydrogen purifier 14, booster fan 12, purity nitrogen gas tank 11, rush nitrogen valve 10 and be sequentially connected by pipeline, the atmosphere of constituent apparatus replaces circuit, while for nitrogenizing；The reactor tank 1 is sequentially connected with cooler 2, reduction air outlet valve 3, clarifier 4, reduction gas-reservoir tank 6, booster fan 5, mixer 8, reduction intake valve 9 by pipeline, the reduction circuit of constituent apparatus.The present invention has heat utilization rate high, and heat load adjustment is fast, and high production efficiency, electricity consumption is few, and production cost is low, and product effective content is high, and host element nitrogen, manganese and value are up to 99% or more.
Description
Technical field
The present invention relates to the production fields of additive nitrogenized manganese in Ferrous Metallurgy, and in particular to the production of high purity silicon nitride manganese
Technology.
Background technique
Demand of the development of special steel to nitrogenized manganese increases, especially high to nitrogen and manganese element content, other impurities element
The low high-quality nitrogenized manganese demand of content is more.
It is currently suggested the production method of many nitrogenized manganeses, used nitridation equipment has tube furnace, fluidized-bed reaction
Furnace, rotary furnace etc.；Pressurization (nitridation pressure be greater than 0.1 MPa), 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 resistance nitridation of the patent No. 200910044526.9
Furnace), the yield of annual nitrogenized manganese has more than ten thousand tons, obtains preferable economic benefit, however there is also following disadvantages.
(1) it is directly heated using carbon electrode, carbon material can volatilize evolution, penetrate into product, polluted product makes product
Carbon is easy exceeded.
(2) process units energy consumption is higher, and technique requires the condition of high vacuum degree of 10Pa before 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
It is up to 10~12 hours, time-consuming to consume energy again, while furnace shell temperature distortion in order to prevent, it is provided with stove outer covering water spray system, band
Amount of heat is walked, comprehensive 750 DEG C of the power consumption of device product per ton early period, for later period device by improving, comprehensive power consumption also there are 500 DEG C.
(3) whole device fixed investment is high, and every furnace production cycle is up to 40~48 hours.Pure nitrogen gas utilization rate is low, scale
Metaplasia is lost greatly in producing.
Also there is technical solution to propose to rush the nitrogenous reducibility gas such as ammonia or ammonia pyrolysis gas into furnace, reaction production water could not and
When be discharged, vapor partial pressure is high, is unfavorable for continuing for reduction reaction, most manganese oxide could not restore.
Summary of the invention
It is an object of the invention to overcome deficiency existing for above-mentioned technology, a kind of novel high purity silicon nitride manganese production dress is provided
It sets, removes the reducibility oxygen in raw material, improve the quality of product, reduce the time consumption and energy consumption in production.
Technical scheme is as follows: a kind of novel high purity silicon nitride manganese process units mainly adds including regenerative gas
Hot stove, reactor tank, cooler, rough vacuum pump plus hydrogen purifier, rich nitrogen gas tank, reduction gas-reservoir tank, mixer, the reactor tank
With cooler, pump intake valve, rough vacuum pump, pump out air valve, rich nitrogen basin plus hydrogen purifier, booster fan, purity nitrogen gas tank,
It rushes nitrogen valve to be sequentially connected by pipeline, the atmosphere of constituent apparatus replaces circuit, while for nitrogenizing；The reactor tank and cooling
Device, reduction air outlet valve, clarifier, reduction gas-reservoir tank, booster fan, mixer, reduction intake valve are sequentially connected by pipeline, structure
At the reduction circuit of device.
Further, reverting back on road in device, the mixer have branched pipe to be connected with ammonia cracker, for supplementing also
Former hydrogen, the mixer separately have branch pipe with plus hydrogen purifier be connected, add hydrogen to purify to provide hydrogen for rich nitrogen.
Further, on the atmosphere displacement circuit of device, the pure nitrogen gas basin is connected by pipeline with nitrogen making machine, described
Rough vacuum pump outlet conduit is equipped with exhaust-valve, the cooler outlet pipe be equipped with moisture detector and oxygen, hydrogen detector and
Safe draining valve.
Further, the reactor tank is placed in regenerative gas heating furnace, and reactor tank both ends are outside furnace, regenerative gas
Heating furnace is provided with heat-accumulating burner and four-way reversing valve, makes into furnace combustion gas and kiln gas carries out sufficient heat exchange out, thermal energy obtains
To making full use of.
Further, the reactor tank both ends are equipped with water leg and thermal radiation resistant isolation board, and the material of reactor tank is high temperature resistant
High strength alloy steel, 300~420mm of diameter of reactor tank, 2000~4000mm of length, 30~60mm of wall thickness pass through centrifugal casting
It makes to obtain, is usually used in magnesium smelting reduction pot.
The beneficial effects of the invention are as follows.
1, using regenerative gas heating furnace, heat utilization rate is high, and heat load adjustment is fast, and high production efficiency, electricity consumption is few, raw
It produces at low cost.
2, product effective content is high, and host element nitrogen, manganese and value are up to 99% or more.
3, reactor tank has that volume is big, can account for total measurement (volume) 80%, and the production cycle of product shortens, and passes through atmosphere in reactor tank
Oxygen content in reactor tank, can be down to 0.5% in 2 hours, the production cycle of a batch products can be controlled in 12 hours by displacement
It is interior.
4, for rich nitrogen by adding hydrogen to purify, nitrogen utilization rate is high.
Detailed description of the invention:
Fig. 1 is production equipment connection figure of the invention.
Specific embodiment:
Illustrate below with reference to Fig. 1 to the present invention: a kind of novel high purity silicon nitride manganese process units mainly includes accumulation of heat
Formula gas-fired heater 21, reactor tank 1, cooler 2, rough vacuum pump 19 plus hydrogen purifier 14, rich nitrogen gas tank 16, reduction gas-reservoir tank
6, mixer 8, the reactor tank 1 and cooler 2, pump intake valve 22, rough vacuum pump 19, pump out air valve 17, rich nitrogen basin 16,
Add hydrogen purifier 14, booster fan 12, purity nitrogen gas tank 11, rush nitrogen valve 10 and be sequentially connected by pipeline, the atmosphere of constituent apparatus is set
Road is gained, while for nitrogenizing；The reactor tank 1 and cooler 2, reduction air outlet valve 3, clarifier 4, reduction gas-reservoir tank 6, pressurization
Blower 5, mixer 8, reduction intake valve 9 are sequentially connected by pipeline, the reduction circuit of constituent apparatus.
Further, reverting back on road in device, the mixer 8 has branched pipe to be connected with ammonia cracker 7, for supplementing
Reduction use hydrogen, the mixer 8 separately have branch pipe and plus hydrogen purifier 14 be connected, for richness nitrogen add hydrogen purify hydrogen is provided.
Further, on the atmosphere displacement circuit of device, the pure nitrogen gas basin 11 is connected by pipeline with nitrogen making machine 13,
19 outlet conduit of rough vacuum pump is equipped with exhaust-valve 18,2 outlet of cooler be equipped with moisture detector 24 and oxygen,
Hydrogen detector 25 and safe draining valve 23.
Further, the reactor tank 1 is placed in regenerative gas heating furnace 21, and 1 both ends of reactor tank are outside furnace, the storage
Hot type gas-fired heater 21 is provided with heat-accumulating burner 20 and four-way reversing valve 15, make into furnace combustion gas and out kiln gas carry out it is sufficient
Heat exchange, thermal energy are fully used.
Further, 1 both ends of reactor tank are equipped with water leg and thermal radiation resistant isolation board, and the material of reactor tank is high temperature resistant
High strength alloy steel is obtained by centrifugal casting, is usually used in magnesium-smelting silicothermic process reductive jar, and the diameter 300 of reactor tank~
420mm, 2000~4000mm of length, 30~60mm of wall thickness.
Specific work process of the invention is as follows:
The first step, charge sealed cans, the raw materials such as electrolytic manganese metal piece or manganese powder is packed into reactor tank 1, sealed shell of tank.
Second step, atmosphere displacement:
(a) primary to evacuate exhaust: quickly to take out gas in reactor tank 1 with rough vacuum pump 19, gas bleeding emptying is evacuated to absolute pressure
Pure nitrogen gas is poured into reactor tank 1 after 0.05MPa, after pressure reaches 0.2MPa, nitrogen is rushed in stopping, by gas in reactor tank 1
It is discharged to rich nitrogen basin 16.
(b) secondary evacuation recycling: continuing for reactor tank 1 to be evacuated to rich nitrogen basin 16, after being evacuated to 0.05 MPa of absolute pressure,
Stop rushing nitrogen after rushing pure nitrogen gas to 0.2 MPa of pressure into reactor tank 1 again, gas in reactor tank 1 is discharged to rich nitrogen and is store
Tank 16.
(c) recycling: the b that repeats the above steps operation is evacuated three times, when oxygen, hydrogen detector 25 check that the oxygen content in exhaust is low
In 0.5% hereinafter, completing displacement.
(d) add hydrogen purification: the rich nitrogen for being recovered to rich nitrogen basin 16 is carried out with ammonia pyrolysis gas plus hydrogen is purified, and passes through
Purification after generating water except dereaction, obtains pure nitrogen gas, stores reuse.
Third step starts to start regenerative gas heating furnace 21, regenerative gas heating furnace 21 when carrying out second step
It is provided with heat-accumulating burner 20 and four-way reversing valve 15, makes into furnace combustion gas and kiln gas carries out sufficient heat exchange out, thermal energy obtains
It makes full use of.
4th step, when in-furnace temperature is raised to 800 DEG C.
(a) it is passed through also Primordial Qi, wherein hydrogen content 30~50%, surplus are nitrogen, maintain 0.05 MPa of pressure, temperature 850
~950 DEG C, discharge gas hydrogen content maintains continuous 20~30%, and discharge air cooling purification is recovered to reduction gas-reservoir tank 6, and examined with moisture
It surveys instrument 24 and detects gas moisture content.
(b) when outlet moisture content is less than 0.1g/Nm3When, 90% or more combination oxygen in manganese oxide is reduced, and is changed and is passed through
Pure nitrogen gas, discharge air cooling purify, are recovered to reduction gas-reservoir tank 6, when oxygen, hydrogen detector 25 detect outlet hydrogen content less than 2%
When stop discharge gas.
5th step, nitridation continue to rush pure nitrogen gas, maintain 0.2 MPa of pressure in reactor tank 1, and 950~1050 DEG C of temperature, 4~
6 hours, it is ensured that higher nitrogen partial pressure, Accelerate nitriding reaction promote nitrogen content in manganese.
6th step, pressure maintaining cooling, keeps 0.2 MPa of pressure, stops heating, cooling.
7th step, nitrogen protection is cooling, and when temperature drops to 500 DEG C, pressure release opens flange, discharging to cooling to normal pressure
Tank rushes nitrogen into tank, and product is made to be cooled to 200 DEG C or less under nitrogen protection.
Basic principles and main features of the invention have been shown and described above.It should be understood by those skilled in the art that
The present invention is not limited to the above embodiments, and the above embodiments and description only illustrate the principle of the present invention,
Without departing from the spirit and scope, various changes and improvements may be made to the invention, these changes and improvements are all fallen
Enter in scope of the claimed invention.The scope of the present invention is defined by the appended claims and its equivalents.
Claims (2)
1. a kind of high purity silicon nitride manganese process units, which is characterized in that mainly include regenerative gas heating furnace (21), reactor tank
(1), cooler (2), rough vacuum pump (19) plus hydrogen purifier (14), rich nitrogen gas tank (16), reduction gas-reservoir tank (6), mixer
(8), the reactor tank (1) and cooler (2), pump intake valve (22), rough vacuum pump (19), pump out air valve (17), rich nitrogen gas tank
(16), plus hydrogen purifier (14), booster fan (12), purity nitrogen gas tank (11), rush nitrogen valve (10) and be sequentially connected by pipeline, constitute
The atmosphere of device replaces circuit；The reactor tank (1) and cooler (2), reduction air outlet valve (3), clarifier (4), reduction gas-reservoir
Tank (6), booster fan (5), mixer (8), reduction intake valve (9) are sequentially connected by pipeline, the reduction circuit of constituent apparatus；
The mixer (8) has branched pipe to be connected with ammonia cracker (7), and the mixer (8) separately has branch pipe and plus hydrogen purifier
(14) it is connected；
The purity nitrogen gas tank (11) is connected by pipeline with nitrogen making machine (13), and rough vacuum pump (19) outlet conduit is equipped with row
Empty valve (18), cooler (2) outlet are equipped with moisture detector (24) and oxygen, hydrogen detector (25) and safe draining valve
(23)；
The reactor tank (1) is placed in regenerative gas heating furnace (21), and reactor tank (1) both ends are outside furnace, regenerative gas
Heating furnace (21) is provided with heat-accumulating burner (20) and four-way reversing valve (15).
2. a kind of high purity silicon nitride manganese process units according to claim 1, which is characterized in that reactor tank (1) both ends
Equipped with water leg and thermal radiation resistant isolation board, the material of reactor tank is high temperature resistance and high strength alloy steel, is obtained by centrifugal casting,
300~420mm of diameter of reactor tank, 2000~4000mm of length, 30~60mm of wall thickness.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710439129.6A CN107140611B (en) | 2017-06-13 | 2017-06-13 | A kind of novel high purity silicon nitride manganese process units |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710439129.6A CN107140611B (en) | 2017-06-13 | 2017-06-13 | A kind of novel high purity silicon nitride manganese process units |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107140611A CN107140611A (en) | 2017-09-08 |
| CN107140611B true CN107140611B (en) | 2019-03-08 |
Family
ID=59782353
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710439129.6A Active CN107140611B (en) | 2017-06-13 | 2017-06-13 | A kind of novel high purity silicon nitride manganese process units |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107140611B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109198654A (en) * | 2018-11-08 | 2019-01-15 | 河南工业大学 | A kind of equipment for extracting dietary fiber from wheat bran |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2289990A (en) * | 1939-05-18 | 1942-07-14 | Alfred P Parker | Manufacture of hollow articles |
| US2860080A (en) * | 1956-06-06 | 1958-11-11 | Foote Mineral Co | Method for continuously producing thermally-stable nitrided manganese |
| CN101172586A (en) * | 2007-09-30 | 2008-05-07 | 冯良荣 | Method for producing manganese nitride |
| CN103601160A (en) * | 2013-11-29 | 2014-02-26 | 湖南源创高科工业技术有限公司 | Preparation method of manganese nitride |
| CN103614582A (en) * | 2013-12-13 | 2014-03-05 | 东北大学 | Method for producing manganese nitride product |
| CN103849829A (en) * | 2012-12-03 | 2014-06-11 | 安徽港铭新材料科技有限公司 | Preparation method for manganese-nitrogen alloy |
-
2017
- 2017-06-13 CN CN201710439129.6A patent/CN107140611B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2289990A (en) * | 1939-05-18 | 1942-07-14 | Alfred P Parker | Manufacture of hollow articles |
| US2860080A (en) * | 1956-06-06 | 1958-11-11 | Foote Mineral Co | Method for continuously producing thermally-stable nitrided manganese |
| CN101172586A (en) * | 2007-09-30 | 2008-05-07 | 冯良荣 | Method for producing manganese nitride |
| CN103849829A (en) * | 2012-12-03 | 2014-06-11 | 安徽港铭新材料科技有限公司 | Preparation method for manganese-nitrogen alloy |
| CN103601160A (en) * | 2013-11-29 | 2014-02-26 | 湖南源创高科工业技术有限公司 | Preparation method of manganese nitride |
| CN103614582A (en) * | 2013-12-13 | 2014-03-05 | 东北大学 | Method for producing manganese nitride product |
Non-Patent Citations (2)
| Title |
|---|
| "基于粉末压坯的氮化锰制备技术";吴庆定等;《金属热处理》;20070925;第32卷(第9期);第5-8页 |
| "氮化锰制备工艺研究进展";陈珏俐;《铁合金》;20111228(第6期);第44-48页 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107140611A (en) | 2017-09-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103882246B (en) | Vacuum magnesium manufacturing device and vacuum magnesium manufacturing method | |
| CN102173424B (en) | Method and equipment for removing phosphorus and metal impurities in ganister sand through vacuum induction melting | |
| CN102923699B (en) | Continuous pyrographite purifying device | |
| CN102992285A (en) | Method and equipment for producing yellow phosphorus by utilizing closed annular heating furnace | |
| CN107140611B (en) | A kind of novel high purity silicon nitride manganese process units | |
| CN109913606A (en) | A kind of coal hydrogen shaft furnace ironmaking system and technique based on induction heating | |
| CN101294239B (en) | Reutilization method for annealing oven protective atmosphere | |
| CN104101225B (en) | For improving the system and method for calcium carbide stove exhaust comprehensive utilization ratio | |
| CN201292397Y (en) | Vacuum metallurgy furnace suitable for producing magnesium metal with carbon thermoreduction of magnesium oxide | |
| CN103160698B (en) | Vanadium nitride alloy production technology | |
| CN107416779A (en) | A kind of energy-efficient high purity silicon nitride manganese process units | |
| CN107986279A (en) | A kind of microwave furnace of calcium carbide reactor and prepare the method for calcium carbide using it | |
| CN105399106B (en) | The preparation method and device of a kind of high purity boron powder | |
| CN107140610B (en) | A kind of energy-efficient high purity silicon nitride manganese production method | |
| CN207209961U (en) | A kind of energy-efficient high purity silicon nitride manganese production system | |
| CN212293673U (en) | Nitrogen recycling device for use in heat preservation period of bell-type annealing furnace | |
| CN107010610A (en) | A kind of energy-efficient high purity silicon nitride manganese production system | |
| CN101709916A (en) | Multi-functional environment-protection smelting furnace of low energy consumption silicon carbide (or other metal and nonmetal) and process | |
| CN206918977U (en) | Magnesium metal smelt reducing slag waste-heat recovery device | |
| CN102994785B (en) | Method for smelting hydrogen storage alloy containing titanium from BaZrO3 refractory material by vacuum induction | |
| CN103058197A (en) | Vacuum circulation solar-grade polycrystalline silicon refining equipment and solar-grade polycrystalline silicon refining method | |
| CN101994083A (en) | Method for producing ferrochrome nitride with microwave as heat source | |
| CN105483330A (en) | Vacuum system for vacuum degassing smelting furnace, and control method thereof | |
| CN104773714A (en) | Method for continuously producing manganese nitride product | |
| CN103882186A (en) | Vacuum-pumping device of RH (Ruhrstahl Hereaeus) refining furnace and use method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20190124 Address after: 416000 Industrial Avenue of Xiangxi Economic Development Zone, Xiangxi Tujia and Miao Autonomous Prefecture, Hunan Province (beside Fengda Alloy Technology Co., Ltd. of Xiangxi Autonomous Prefecture) Applicant after: Xiangxi Autonomous Prefecture Rong Hua new materials Co., Ltd. Address before: 416400 Public Security Village No. 51, Huayuan Town, Huayuan County, Tujia and Miao Autonomous Prefecture, Western Hunan Province Applicant before: Wang Zhaobing |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant |