CN106865507A - A kind of method that utilization ammonium poly-vanadate directly prepares vanadium nitride - Google Patents
A kind of method that utilization ammonium poly-vanadate directly prepares vanadium nitride Download PDFInfo
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- CN106865507A CN106865507A CN201710097409.3A CN201710097409A CN106865507A CN 106865507 A CN106865507 A CN 106865507A CN 201710097409 A CN201710097409 A CN 201710097409A CN 106865507 A CN106865507 A CN 106865507A
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- 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
- C01B21/0615—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 transition metals other than titanium, zirconium or hafnium
- C01B21/0617—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 transition metals other than titanium, zirconium or hafnium with vanadium, niobium or tantalum
Abstract
The invention discloses a kind of method that utilization ammonium poly-vanadate directly prepares vanadium nitride, the step is as follows：Wet basis ammonium poly-vanadate is dried, block butt ammonium poly-vanadate is obtained, mixed material is mixed to get with graphite carbon dust, binding agent poly-vinyl alcohol solution, catalyst metals iron powder after grinding, mixed material carries out preforming compacting, obtains preforming material；The preforming material is put into graphite batch can be placed in nitridation kiln and carries out reduction nitridation, vanadium nitride is obtained after cooling.This method preparation process is simple, directly vanadium nitride can be prepared by by raw material of ammonium poly-vanadate, obtained vanadium nitride nitrogen content is higher, and the ammonia that ammonium poly-vanadate is decomposed is used as reaction raw materials, the auxiliary material needed during production is few, energy consumption is low, low production cost, with preferable market prospects.
Description
Technical field
The invention belongs to vanadium nitride preparing technical field, and in particular to a kind of utilization ammonium poly-vanadate directly prepares vanadium nitride
Method.
Background technology
Vanadium is a kind of important alloying element in steel production, and its application in low micro alloyed steel is widely.
VN alloy is a kind of novel alloy additive, can substitute vanadium iron for the production of micro alloyed steel, and vanadium nitride makes an addition to steel
The comprehensive mechanical performances such as the middle intensity that can improve steel, toughness, ductility and thermal fatigue resistance, and it is good solderable to have steel
Property, in the case where same intensity is reached, addition vanadium nitride saves vanadium addition 30-40%, and then reduces cost.In recent years, due to vanadium
The obvious technology of nitrogen micro-alloying technology and economic advantages so that vanadium nitrogen microalloy is in high strength cast iron, non-hardened and tempered steel, high intensity
It is widely used in the development ＆ production of product such as strip, high-strength plank and heavy wall H profile steel, seamless steel pipe, tool steel.
Especially in the gradually popularization of China, the development of VN alloy technology also achieves tangible result.Existing vanadium nitride life
Production. art is main to carry out reduction nitridation by raw material of vanadic anhydride or vanadium trioxide, and processing step is cumbersome, in the mistake of production
The vanadium raw materials that are used in journey are expensive, the consumption of course of reaction energy consumption is big, the production cycle is long.Therefore, life is used conventional methods
The next vanadium nitride of output is relatively costly, the market competitiveness is low.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of method that utilization ammonium poly-vanadate directly prepares vanadium nitride.This hair
The bright ammonium poly-vanadate that realizes directly prepares vanadium nitride, makes full use of accessory substance, simple production process, low cost.
To solve the above problems, the present invention is adopted the following technical scheme that：One kind directly prepares nitridation using ammonium poly-vanadate
The method of vanadium, the step is as follows：1）Wet basis ammonium poly-vanadate is dried, block butt ammonium poly-vanadate is obtained；2）Described piece
It is mixed to get and mixes with graphite carbon dust, binding agent poly-vinyl alcohol solution, catalyst metals iron powder after the grinding of shape butt ammonium poly-vanadate
Material；3）The mixed material carries out preforming compacting, obtains preforming material；4）The preforming material is put into graphite material
Being placed in tank in nitridation kiln carries out reduction nitridation, and vanadium nitride is obtained after cooling.
Step 1 of the present invention）The weight/mass percentage composition of middle wet basis ammonium poly-vanadate main component is as follows：H2O：10~15%,
V2O5：65~70%, Fe：5~10%, Si:0.5~1.0%, P：0.006~0.01%, S：0.05~0.1%, K2O+Na2O content is
0.3~0.8%.
Step 1 of the present invention）Wet basis ammonium poly-vanadate is dried treatment, and drying temperature is 80~150 DEG C, drying time
Butt ammonium poly-vanadate is obtained after 4~8h, the grinding of butt ammonium poly-vanadate is in powdery, standby after the mesh of granularity≤200.
Step 2 of the present invention）Butt ammonium poly-vanadate is 4 with graphite carbon dust in mass ratio:1~8:1, graphite carbon dust with urge
Agent mass ratio is 1:0.005~1:0.1, it is sufficiently mixed uniform rear standby.
Step 2 of the present invention）Graphite carbon dust is reducing agent, granularity≤200 mesh, purity >=98%；The catalyst is gold
Category iron powder, granularity≤100 mesh, purity >=99%.
Step 2 of the present invention）The quality of binding agent addition is the 5~25% of butt ammonium poly-vanadate quality；The binding agent
It is poly-vinyl alcohol solution, polyvinyl alcohol weight/mass percentage composition is 2~5%.
Step 3 of the present invention）Stress control is in 10~20Mpa, the preform for obtaining during material is compressing
Material is in ball-type, its a diameter of 45~60mm.
Step 4 of the present invention）In preforming material be put in porous batch can, material and batch can are together put in nitridation kiln
Reduction nitridation is inside carried out, vanadium nitride is obtained.
Step 4 of the present invention）In nitridation kiln in reduction nitridation step, kiln cavity pressure is 5~20Pa, anti-in nitridation kiln
It is 1450~1650 DEG C to answer temperature, and nitridation time is 10~25h.
Step 4 of the present invention）After reduction nitridation reaction terminates, material cooling section in kiln is lowered the temperature, and temperature is less than
Kiln discharge after 50 DEG C, obtains vanadium nitride, described 77.5~79.5wt% of vanadium nitride vanadium content, the vanadium nitride of nitrogenous >=10wt%；It is close
Degree >=3.5g/cm3。
It is using the beneficial effect produced by above-mentioned technical proposal：Directly carried out as containing vanadium raw materials using ammonium poly-vanadate
Production vanadium nitride, makes the gas-solid reaction contact area that effectively increases in course of reaction of ammonia that raw material decomposes are produced, beneficial to oozing
Nitrogen reacts, while after material is directly entered high-temperature region, accessory substance is utilized as nitrogen-containing material during reduction nitridation, can be with
The consumption of graphite carbon dust and nitrogen is effectively reduced, product quality is effectively increased.Ammonium poly-vanadate is realized in the present invention directly to make
Standby vanadium nitride, makes full use of accessory substance, with process is simple, low cost, it is good in economic efficiency the features such as.
Specific embodiment
The processing step that the method for vanadium nitride is directly prepared using ammonium poly-vanadate is：
（1）As containing vanadium raw materials after being dried using wet basis ammonium poly-vanadate.
（2）Wet basis ammonium poly-vanadate is dried, drying temperature is 80~150 DEG C, 4~8h of drying time obtains block dry
Quito ammonium vanadate, is mixed after being ground with graphite carbon dust, binding agent, catalyst.
（3）The powdered vanadium-containing material of described butt is 4 with graphitic carbon powder mass ratio:1~8:1, graphite carbon dust with catalysis
Agent mass ratio is 1：0.05~1:0.2, the material of addition is 10 with the binding agent mass ratio of addition:1~20:1, it is sufficiently mixed
Carry out preforming compressing after even, obtain the ball-type material of a diameter of 45~60mm as the raw material of reduction-nitridation.
（4）Preforming material and batch can are together put into nitridation kiln carries out high temperature reduction nitridation, the nitridation kiln furnace chamber
Interior pressure is 5~20Pa, and nitridation kiln interior reaction temperature is 1450~1650 DEG C, and nitridation time is 10~25h, obtains vanadium nitride.
With reference to specific embodiment, the present invention is further detailed explanation, being selected from containing vanadium raw materials in embodiment：
The wet basis ammonium vanadate of acid ammonium salt precipitation process industry production；The weight/mass percentage composition of its main component is as follows：H2O：10~
15%, V2O5：65~70%, Fe：10~15%, Si:0.5~1.0%, P：0.006~0.01%, S：0.05~0.1%, K2O+Na2O
Content is 0.3~0.8%.
Embodiment 1
A kind of method that utilization ammonium poly-vanadate directly prepares vanadium nitride, the step is as follows：
1）Wet basis ammonium poly-vanadate is dried 8h at 80 DEG C, block butt ammonium poly-vanadate is obtained, grinding is in granularity≤200 mesh powder
Shape is standby；
The weight/mass percentage composition of wet basis ammonium poly-vanadate main component is as follows：H2O：14%, V2O5：69.5%, Fe：15%, Si:0.6%,
P：0.009%, S：0.07%, K2O+Na2O content is 0.6%.
2）The block butt ammonium poly-vanadate powder 1000g, graphite carbon dust 150g, binding agent poly-vinyl alcohol solution 100g,
Catalyst metals iron powder 3g, well mixed to obtain mixed material, binding agent is the poly-vinyl alcohol solution of weight/mass percentage composition 5%；
Graphite carbon dust is reducing agent, granularity≤200 mesh, purity >=98%；Catalyst is metal iron powder, granularity≤100 mesh, purity
≥99%。
3）The mixed material carries out preforming compacting, and pressing pressure is 10Mpa, obtains the ball-type of a diameter of 45~60mm
Preforming material；
4）The preforming material is put into the porous batch can of graphite, material is together put in nitridation kiln with batch can and is reduced
Nitridation is placed in and reduction nitridation is carried out in nitridation kiln, and kiln cavity pressure is 15Pa, and nitridation kiln interior reaction temperature is 1450 DEG C, during nitridation
Between be 15h；After reduction nitridation reaction terminates, material cooling section in kiln is lowered the temperature, and kiln discharge after 31 DEG C of temperature is nitrogenized
Vanadium.
Described vanadium nitride product main chemical compositions content is as follows：V：77.98%, N：12.52%, C：6.89%, P：
0.06%, S：0.04%.Vanadium nitride apparent density is 3.51g/cm3, the vanadium nitride qualification rate 100% for obtaining, system vanadium yield is
96.5%。
Embodiment 2
A kind of method that utilization ammonium poly-vanadate directly prepares vanadium nitride, the step is as follows：
1）Wet basis ammonium poly-vanadate is dried 5h at 100 DEG C, block butt ammonium poly-vanadate is obtained, grinding is in granularity≤200 mesh
Powdery is standby；
The weight/mass percentage composition of wet basis ammonium poly-vanadate main component is as follows：H2O：13.5%, V2O5：70%, Fe：15%, Si:0.5%,
P：0.009%, S：0.08%, K2O+Na2O content is 0.3%.
2）The block butt ammonium poly-vanadate powder 1000g, graphite carbon dust 200g, binding agent poly-vinyl alcohol solution 100g,
Catalyst metals iron powder 2.0g, well mixed to obtain mixed material, binding agent is molten for the polyvinyl alcohol of weight/mass percentage composition 2.5%
Liquid；
Graphite carbon dust is reducing agent, granularity≤200 mesh, purity >=98%；Catalyst is metal iron powder, granularity≤100 mesh, purity
≥99%。
3）The mixed material carries out preforming compacting, and pressing pressure is 10Mpa, obtains the ball-type of a diameter of 45~60mm
Preforming material；
4）The preforming material is put into the porous batch can of graphite, material is together put in nitridation kiln with batch can and is reduced
Nitridation is placed in and reduction nitridation is carried out in nitridation kiln, and kiln cavity pressure is 15Pa, and nitridation kiln interior reaction temperature is 1550 DEG C, during nitridation
Between be 20h；After reduction nitridation reaction terminates, material cooling section in kiln is lowered the temperature, and kiln discharge after 41 DEG C of temperature is nitrogenized
Vanadium.
Described vanadium nitride product main chemical compositions content is as follows：V：78.02%, N：13.52%, C：6.31%, P：
0.06%, S：0.04%.Vanadium nitride apparent density is 3.5g/cm3, the vanadium nitride qualification rate 100% for obtaining, system vanadium yield is
96.3%。
Embodiment 3
A kind of method that utilization ammonium poly-vanadate directly prepares vanadium nitride, the step is as follows：
1）Wet basis ammonium poly-vanadate is dried 5h at 90 DEG C, block butt ammonium poly-vanadate is obtained, grinding is in granularity≤200 mesh powder
Shape is standby；
The weight/mass percentage composition of wet basis ammonium poly-vanadate main component is as follows：H2O：14.5%, V2O5：69%, Fe：15%, Si:0.6%,
P：0.007%, S：0.07%, K2O+Na2O content is 0.4%.
2）The block butt ammonium poly-vanadate powder 1000g, graphite carbon dust 200g, binding agent poly-vinyl alcohol solution 100g,
Catalyst metals iron powder 2g, well mixed to obtain mixed material, binding agent is the poly-vinyl alcohol solution of weight/mass percentage composition 3%；
Graphite carbon dust is reducing agent, granularity≤200 mesh, purity >=98%；Catalyst is metal iron powder, granularity≤100 mesh, purity
≥99%。
3）The mixed material carries out preforming compacting, and pressing pressure is 20Mpa, obtains the ball-type of a diameter of 45~60mm
Preforming material；
4）The preforming material is put into the porous batch can of graphite, material is together put in nitridation kiln with batch can and is reduced
Nitridation is placed in and reduction nitridation is carried out in nitridation kiln, and kiln cavity pressure is 15Pa, and nitridation kiln interior reaction temperature is 1500 DEG C, during nitridation
Between be 25h；After reduction nitridation reaction terminates, material cooling section in kiln is lowered the temperature, and kiln discharge after 35 DEG C of temperature is nitrogenized
Vanadium.
Described vanadium nitride product main chemical compositions content is as follows：V：78.02%, N：14.52%, C：5.11%, P：
0.02%, S：0.1%.Vanadium nitride apparent density is 3.53g/cm3, the vanadium nitride qualification rate 100% for obtaining, system vanadium yield is
96.4%。
Embodiment 4
A kind of method that utilization ammonium poly-vanadate directly prepares vanadium nitride, the step is as follows：
1）Wet basis ammonium poly-vanadate is dried 5h at 100 DEG C, block butt ammonium poly-vanadate is obtained, grinding is in granularity≤200 mesh
Powdery is standby；
The weight/mass percentage composition of wet basis ammonium poly-vanadate main component is as follows：H2O：13.5%, V2O5：70%, Fe：15%, Si:0.8%,
P：0.009%, S：0.08%, K2O+Na2O content is 0.3%.
2）The block butt ammonium poly-vanadate powder 1000g, graphite carbon dust 200g, binding agent poly-vinyl alcohol solution 200g,
Catalyst metals iron powder 1.5g, well mixed to obtain mixed material, binding agent is the poly-vinyl alcohol solution of weight/mass percentage composition 2%；
Graphite carbon dust is reducing agent, granularity≤200 mesh, purity >=98%；Catalyst is metal iron powder, granularity≤100 mesh, purity
≥99%。
3）The mixed material carries out preforming compacting, and pressing pressure is 20Mpa, obtains the ball-type of a diameter of 45~60mm
Preforming material；
4）The preforming material is put into the porous batch can of graphite, material is together put in nitridation kiln with batch can and is reduced
Nitridation is placed in and reduction nitridation is carried out in nitridation kiln, and kiln cavity pressure is 15Pa, and nitridation kiln interior reaction temperature is 1550 DEG C, during nitridation
Between be 25h；After reduction nitridation reaction terminates, material cooling section in kiln is lowered the temperature, and kiln discharge after 38 DEG C of temperature is nitrogenized
Vanadium.
Described vanadium nitride product main chemical compositions content is as follows：V：78.92%, N：15.31%, C：4.11%, P：
0.05%, S：0.1%.Vanadium nitride apparent density is 3.55g/cm3, the vanadium nitride qualification rate 100% for obtaining, system vanadium yield is
96.3%。
Embodiment 5
A kind of method that utilization ammonium poly-vanadate directly prepares vanadium nitride, the step is as follows：
1）Wet basis ammonium poly-vanadate is dried 4h at 110 DEG C, block butt ammonium poly-vanadate is obtained, grinding is in granularity≤200 mesh
Powdery is standby；
The weight/mass percentage composition of wet basis ammonium poly-vanadate main component is as follows：H2O：14.3%, V2O5：70.0%, Fe：14.5%, Si:
0.7%, P：0.006%, S：0.07%, K2O+Na2O content is 0.4%.
2）The block butt ammonium poly-vanadate powder 1000g, graphite carbon dust 150g, binding agent poly-vinyl alcohol solution 150g,
Catalyst metals iron powder 15g, well mixed to obtain mixed material, binding agent is the poly-vinyl alcohol solution of weight/mass percentage composition 5%；
Graphite carbon dust is reducing agent, granularity≤200 mesh, purity >=98%；Catalyst is metal iron powder, granularity≤100 mesh, purity
≥99%。
3）The mixed material carries out preforming compacting, and pressing pressure is 15Mpa, obtains the ball-type of a diameter of 45~60mm
Preforming material；
4）The preforming material is put into the porous batch can of graphite, material is together put in nitridation kiln with batch can and is reduced
Nitridation is placed in and reduction nitridation is carried out in nitridation kiln, and kiln cavity pressure is 20Pa, and nitridation kiln interior reaction temperature is 1550 DEG C, during nitridation
Between be 25h；After reduction nitridation reaction terminates, material cooling section in kiln is lowered the temperature, and kiln discharge after 36 DEG C of temperature is nitrogenized
Vanadium.
Described vanadium nitride product main chemical compositions content is as follows：V：77.92%, N：12.31%, C：5.61%, P：
0.06%, S：0.11%.Vanadium nitride apparent density is 3.54g/cm3, the vanadium nitride qualification rate 100% for obtaining, system vanadium yield is
96.6%。
Embodiment 6
A kind of method that utilization ammonium poly-vanadate directly prepares vanadium nitride, the step is as follows：
1）Wet basis ammonium poly-vanadate is dried 4h at 150 DEG C, block butt ammonium poly-vanadate is obtained, grinding is in granularity≤200 mesh
Powdery is standby；
The weight/mass percentage composition of wet basis ammonium poly-vanadate main component is as follows：H2O：10.0%, V2O5：69.6%, Fe：10.0%, Si:
0.7%, P：0.008%, S：0.05%, K2O+Na2O content is 0.4%.
2）The block butt ammonium poly-vanadate powder 1000g, graphite carbon dust 250g, binding agent poly-vinyl alcohol solution 50g, urge
Agent metal iron powder 15g, well mixed to obtain mixed material, binding agent is the poly-vinyl alcohol solution of weight/mass percentage composition 4%；
Graphite carbon dust is reducing agent, granularity≤200 mesh, purity >=98%；Catalyst is metal iron powder, granularity≤100 mesh, purity
≥99%。
3）The mixed material carries out preforming compacting, and pressing pressure is 15Mpa, obtains the ball-type of a diameter of 45~60mm
Preforming material；
4）The preforming material is put into the porous batch can of graphite, material is together put in nitridation kiln with batch can and is reduced
Nitridation is placed in and reduction nitridation is carried out in nitridation kiln, and kiln cavity pressure is 15Pa, and nitridation kiln interior reaction temperature is 1550 DEG C, during nitridation
Between be 20h；After reduction nitridation reaction terminates, material cooling section in kiln is lowered the temperature, and kiln discharge after 35 DEG C of temperature is nitrogenized
Vanadium.
Described vanadium nitride product main chemical compositions content is as follows：V：78.02%, N：14.31%, C：4.61%, P：
0.05%, S：0.09%.Vanadium nitride apparent density is 3.51g/cm3, the vanadium nitride qualification rate 100% for obtaining, system vanadium yield is
96.5%。
Embodiment 7
A kind of method that utilization ammonium poly-vanadate directly prepares vanadium nitride, the step is as follows：
1）Wet basis ammonium poly-vanadate is dried 5h at 100 DEG C, block butt ammonium poly-vanadate is obtained, grinding is in granularity≤200 mesh
Powdery is standby；
The weight/mass percentage composition of wet basis ammonium poly-vanadate main component is as follows：H2O：15.0%, V2O5：65.0%, Fe：14.9%, Si:
1.0%, P：0.010%, S：0.10%, K2O+Na2O content is 0.8%.
2）The block butt ammonium poly-vanadate powder 1000g, graphite carbon dust 125g, binding agent poly-vinyl alcohol solution 250g,
Catalyst metals iron powder 0.625g, well mixed to obtain mixed material, binding agent is molten for the polyvinyl alcohol of weight/mass percentage composition 3%
Liquid；
Graphite carbon dust is reducing agent, granularity≤200 mesh, purity >=98%；The catalyst be metal iron powder, granularity≤100 mesh,
Purity >=99%.
3）The mixed material carries out preforming compacting, and pressing pressure is 15Mpa, obtains the ball-type of a diameter of 45~60mm
Preforming material；
4）The preforming material is put into the porous batch can of graphite, material is together put in nitridation kiln with batch can and is reduced
Nitridation is placed in and reduction nitridation is carried out in nitridation kiln, and kiln cavity pressure is 5Pa, and nitridation kiln interior reaction temperature is 1650 DEG C, during nitridation
Between be 10h；After reduction nitridation reaction terminates, material cooling section in kiln is lowered the temperature, and kiln discharge after temperature 50 C is nitrogenized
Vanadium.
Described vanadium nitride product main chemical compositions content is as follows：V：78.02%, N：15.02%, C：4.81%, P：
0.05%, S：0.09%.Vanadium nitride apparent density is 3.57g/cm3, the vanadium nitride qualification rate 100% for obtaining, system vanadium yield is
96.1%。
Above example is only used to illustrative and not limiting technical scheme, although with reference to above-described embodiment to this hair
It is bright to be described in detail, it will be understood by those within the art that：Still the present invention can be modified or be waited
With replacement, any modification or partial replacement without departing from the spirit and scope of the present invention, it all should cover in power of the invention
In the middle of sharp claimed range.
Claims (10)
1. a kind of method that utilization ammonium poly-vanadate directly prepares vanadium nitride, it is characterised in that the step is as follows：
1）Wet basis ammonium poly-vanadate is dried, block butt ammonium poly-vanadate is obtained；
2）With graphite carbon dust, binding agent poly-vinyl alcohol solution, catalyst metals iron powder after the block butt ammonium poly-vanadate grinding
It is mixed to get mixed material；
3）The mixed material carries out preforming compacting, obtains preforming material；
4）The preforming material is put into graphite batch can be placed in nitridation kiln and carries out reduction nitridation, nitrogen is obtained after cooling
Change vanadium.
2. the method that a kind of utilization ammonium poly-vanadate according to claim 1 directly prepares vanadium nitride, it is characterised in that：It is described
Step 1）The weight/mass percentage composition of middle wet basis ammonium poly-vanadate main component is as follows：H2O：15~20%, V2O5：65~70%, Fe：5~
10%, Si:0.5~1.0%, P：0.006~0.01%, S：0.05~0.1%, K2O+Na2O content is 0.3~0.8%.
3. the method that utilization ammonium poly-vanadate according to claim 1 directly prepares vanadium nitride, it is characterised in that：The step
1）Wet basis ammonium poly-vanadate is dried treatment, and drying temperature is 80~150 DEG C, and many vanadic acid of butt are obtained after 4~8h of drying time
Ammonium, butt ammonium poly-vanadate grinding is in powdery, standby after the mesh of granularity≤200.
4. the method that the utilization ammonium poly-vanadate according to claim 1-3 any one directly prepares vanadium nitride, its feature exists
In：The step 2）Butt ammonium poly-vanadate is 4 with graphite carbon dust in mass ratio:1~8:1, graphite carbon dust and catalyst quality ratio
It is 1:0.005~1:0.1, it is sufficiently mixed uniform rear standby.
5. the method that the utilization ammonium poly-vanadate according to claim 1-3 any one directly prepares vanadium nitride, its feature exists
In：The step 2）Graphite carbon dust is reducing agent, granularity≤200 mesh, purity >=98%；The catalyst is metal iron powder, granularity
≤ 100 mesh, purity >=99%.
6. the method that the utilization ammonium poly-vanadate according to claim 1-3 any one directly prepares vanadium nitride, its feature exists
In：The step 2）The quality of binding agent addition is the 5~25% of butt ammonium poly-vanadate quality；The binding agent is polyvinyl alcohol
Solution, polyvinyl alcohol weight/mass percentage composition is 2~5%.
7. the method that the utilization ammonium poly-vanadate according to claim 1-3 any one directly prepares vanadium nitride, its feature exists
In：The step 3）In 10~20Mpa, the preforming material for obtaining is in ball-type to Stress control during material is compressing, its
A diameter of 45~60mm.
8. the method that the utilization ammonium poly-vanadate according to claim 1-3 any one directly prepares vanadium nitride, its feature exists
In：The step 4）In preforming material be put in porous batch can, by material with batch can together be put in nitridation kiln in reduced
Nitridation, is obtained vanadium nitride.
9. the method that the utilization ammonium poly-vanadate according to claim 1-3 any one directly prepares vanadium nitride, its feature exists
In：The step 4）In nitridation kiln in reduction nitridation step, kiln cavity pressure is 5~20Pa, and nitridation kiln interior reaction temperature is
1450~1650 DEG C, nitridation time is 10~25h.
10. the method that the utilization ammonium poly-vanadate according to claim 1-3 any one directly prepares vanadium nitride, its feature exists
In：The step 4）After reduction nitridation reaction terminates, material cooling section in kiln is lowered the temperature, temperature less than kiln discharge after 50 DEG C,
Obtain vanadium nitride, described 77.5~79.5wt% of vanadium nitride vanadium content, the vanadium nitride of nitrogenous >=10wt%；Density >=3.5g/
cm3。
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| CN107381515A (en) * | 2017-08-08 | 2017-11-24 | 陕西科技大学 | A kind of preparation method and product of vanadium nitride elctro-catalyst |
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