CN1843938A

CN1843938A - Method for preparing vanadium pentoxide

Info

Publication number: CN1843938A
Application number: CN 200610046484
Authority: CN
Inventors: 宿素满; 韩忠民
Original assignee: Individual
Current assignee: Individual
Priority date: 2006-04-30
Filing date: 2006-04-30
Publication date: 2006-10-11

Abstract

The invention relates to a method for preparing vanadic anhydride. It comprises following steps: employing ammonium vanadate, vanadic anhydride of technical grade or waste catalyst discharged in sulfuric acid preparation process; treating with ammonium hydroxide, sulfuric acid and ammonium chloride, washing with water; getting fine active vanadic anhydride; removing foreign matter with ammonium hydroxide, calcium hydroxide, sodium aluminate, sodium silicate, sulfuric acid and ammonium chloride; washing with water again; drying; calcing at 670 Deg. C and getting high-purity vanadic anhydride. The invention is characterized in that it makes use of current material to prepare chemical materials urgently needed by industrial production, and saves a large amount of foreigh exchange.

Description

A kind of production method of Vanadium Pentoxide in FLAKES

[technical field]

The present invention relates to a kind of production and contain vanadium butt 50-54%, the production method of the Vanadium Pentoxide in FLAKES of the refining active Vanadium Pentoxide in FLAKES of CL and production purity 〉=99.5% in nitric acid.

[background technology]

At present the Vanadium Pentoxide in FLAKES of selling on the domestic market contains the vanadium butt all below 50%, can not CL in nitric acid, more there is not the high purity vanadic anhydride of purity 〉=99.5%.And the said products that present China Chemical Manufacture is badly in need of can only spend a large amount of foreign exchanges from external import.

[summary of the invention]

The production method that the purpose of this invention is to provide a kind of Vanadium Pentoxide in FLAKES can be produced and contains vanadium butt 50-54%, refining active Vanadium Pentoxide in FLAKES that can CL in nitric acid, and further produce the high purity vanadic anhydride of purity 〉=99.5% on this basis.

The object of the present invention is achieved like this: with ammonium vanadate, the useless catalyst of discharging when technical grade Vanadium Pentoxide in FLAKES or production sulfuric acid is a raw material, at first pure water being put into retort is heated to about 90 ℃, put into raw material, the weight ratio of raw material and water is about 1: 13, when stirring, slowly add solution of ammonium hydroxide, raw material dissolves the back pH value fully and reaches 7-8, filtering and impurity removing matter, filtrate is put into another retort, be heated to 90 ℃, adding concentration while stirring is 1: the reagent of sulfuric acid of 1-2, adition process was controlled at 8-12 minute, make pH value reach 2-3, whole process temperature remains on about 90 ℃, reaction times is 30-40 minute, the solution pH value is reduced to 6-7, carries out centrifuging after reacting completely, and the dry-matter that obtains is put into retort, add 13 times of pure water, be heated to about 90 ℃, add the ammonium chloride of the 2-3% of entry weight while stirring, the reaction times is 10-15 minute, potassium is removed in centrifuging, sodium impurity, put into retort again, the pure water that adds about 60 ℃ stirs washing, and centrifuging has promptly obtained containing vanadium butt 50-54%, CL in nitric acid, the refining active Vanadium Pentoxide in FLAKES of pentoxide content after the calcination 〉=99%.

Above-mentioned refining active Vanadium Pentoxide in FLAKES is put into retort, the pure water that adds about 13 times of weight, be heated to 90 ℃, add the SILVER REAGENT ammonium hydroxide aqueous solution while stirring, the solution pH value reaches 8-9 in jar, and ferrous iron becomes the ferric iron precipitation, add SILVER REAGENT calcium hydroxide again, add while stirring, pH value removes dephosphorization, silicon to 9-10; Look again foreign matter content such as aluminium suitably adds sodium metaaluminate in the raw material, water glass stirs, transfer pH value to 7-8, to carry out centrifuging with SILVER REAGENT sulfuric acid, filtered liquid is put into retort, be heated to 90 ℃, adding concentration while stirring is 1: the SILVER REAGENT sulfuric acid of 1-2, added in lasting 10-12 minute, and pH value reaches 2-3, the insulation reaction time is 30-40 minute, pH value is reduced to 6-7, and is on inspection, incomplete as precipitin reaction, then continuing to add precipitation agent concentration is 1: the SILVER REAGENT sulfuric acid insulation precipitation of 1-2, carry out centrifuging after reacting completely, the gained siccative is put into retort, adds an amount of 5% SILVER REAGENT ammonium chloride solution again and stir in jar, with potassium, the dissolving of impurity such as sodium, centrifuging is put into retort with siccative and is washed, and washes back oven dry calcination, calcination temperature is about 670 ℃, obtains the high purity vanadic anhydride of purity 〉=99.5%.

Advantage of the present invention is to utilize existing raw material to produce to contain vanadium butt 50-54%, can CL in nitric acid, pentoxide content reaches 99% the refining active Vanadium Pentoxide in FLAKES and the high purity vanadic anhydride of purity 〉=99.5% after the calcination, substitutes import, satisfies the needs of domestic Chemical Manufacture.

[embodiment]

With ammonium vanadate, the useless catalyst of discharging when technical grade Vanadium Pentoxide in FLAKES or production sulfuric acid is a raw material, at first pure water being put into retort is heated to about 90 ℃, put into raw material, the weight ratio of raw material and water is about 1: 13, when stirring, slowly add solution of ammonium hydroxide, raw material dissolves the back pH value fully and reaches 7-8, filtering and impurity removing matter, filtrate is put into another retort, be heated to 90 ℃, adding concentration while stirring is 1: the reagent of sulfuric acid of 1-2, adition process was controlled at 8-12 minute, make pH value reach 2-3, whole process temperature remains on about 90 ℃, reaction times is 30-40 minute, the solution pH value is reduced to 6-7, check whether the oxidation precipitation reaction is complete, method is that stoste is put in the glass cylinder and leaves standstill in taking out jar, treat its clarification after, get clear liquor, in clear liquor, drip 2-3 and drip precipitation agent (sulfuric acid), as drip the no turbid phenomenon in place, explanation reacts completely, as reacts incomplete, then continuing to add concentration is 1: the reagent of sulfuric acid of 1-2, till reacting completely, carry out centrifuging after reacting completely, the dry-matter that obtains is put into retort, add 13 times of weight pure water, be heated to about 90 ℃, the ammonium chloride that the companion limit adds the 2-3% of entry weight is stirred on the limit, and the reaction times is 10-15 minute, potassium is removed in centrifuging, sodium impurity, put into retort again, the pure water that adds about 60 ℃ stirs washing, and centrifuging has promptly obtained containing vanadium butt 50-54%, CL in nitric acid, the refining active Vanadium Pentoxide in FLAKES of pentoxide content after the calcination 〉=99%.

Above-mentioned refining active Vanadium Pentoxide in FLAKES is put into retort, the pure water that adds about 13 times of weight, be heated to 90 ℃, add the SILVER REAGENT ammonium hydroxide aqueous solution while stirring, the solution pH value reaches 8-9 in jar, and ferrous iron becomes the ferric iron precipitation, add SILVER REAGENT calcium hydroxide again, add while stirring, pH value removes dephosphorization, silicon to 9-10; Look again foreign matter content such as aluminium suitably adds sodium metaaluminate in the raw material, water glass stirs, transfer pH value to 7-8, to carry out centrifuging with SILVER REAGENT sulfuric acid, filtered liquid is put into retort, be heated to 90 ℃, adding concentration while stirring is 1: the SILVER REAGENT sulfuric acid of 1-2, added in lasting 10-12 minute, pH value reaches 2-3, and the insulation reaction time is 30-40 minute, and pH value is reduced to 6-7, on inspection, incomplete as precipitin reaction, then continuing to add precipitation agent concentration is 1: the SILVER REAGENT sulfuric acid insulation precipitation of 1-2, after reacting completely, carry out centrifuging, the gained siccative is put into retort, in jar, add an amount of 5% SILVER REAGENT ammonium chloride solution again and stir, with potassium, the dissolving of impurity such as sodium, centrifuging, siccative is put into retort to be washed, method for washing is to add about 60 ℃ pure water in jar, stirs after-filtration, washes back oven dry calcination, calcination temperature is about 670 ℃, obtains the high purity vanadic anhydride of purity 〉=99.5%.

Claims

1, a kind of production method of Vanadium Pentoxide in FLAKES, with ammonium vanadate, technical grade Vanadium Pentoxide in FLAKES or useless catalyst are raw material, it is characterized in that at first pure water being put into retort is heated to about 90 ℃, put into raw material, the weight ratio of raw material and water is about 1: 13, when stirring, slowly add solution of ammonium hydroxide, raw material dissolves the back pH value fully and reaches 7-8, filtering and impurity removing matter, filtrate is put into another retort, be heated to 90 ℃, adding concentration while stirring is 1: the reagent of sulfuric acid of 1-2, adition process was controlled at 8-12 minute, make pH value reach 2-3, whole process temperature remains on about 90 ℃, and the reaction times is 30-40 minute, and the solution pH value is reduced to 6-7, carry out centrifuging after reacting completely, the dry-matter that obtains is put into retort, adds the pure water of 13 times of weight, is heated to about 90 ℃, the ammonium chloride that adds the 2-3% of entry weight while stirring, reaction times is 10-15 minute, after the centrifuging, puts into retort again, the pure water that adds about 60 ℃ stirs washing, centrifuging has promptly obtained containing vanadium butt 50-54% again, CL in nitric acid, the refining active Vanadium Pentoxide in FLAKES of pentoxide content after the calcination 〉=99%.

2, the production method of Vanadium Pentoxide in FLAKES as claimed in claim 1, it is characterized in that above-mentioned refining active Vanadium Pentoxide in FLAKES is put into retort, the pure water that adds about 13 times of weight, be heated to 90 ℃, add the SILVER REAGENT ammonium hydroxide aqueous solution while stirring, the solution pH value reaches 8-9 in jar, adds SILVER REAGENT calcium hydroxide again, add while stirring, pH value is to 9-10; Look again foreign matter content such as aluminium suitably adds sodium metaaluminate in the raw material, water glass stirs, transfer pH value to 7-8, to carry out centrifuging with SILVER REAGENT sulfuric acid, filtered liquid is put into retort, be heated to 90 ℃, adding concentration while stirring is 1: the SILVER REAGENT sulfuric acid of 1-2, added in lasting 10-12 minute, pH value reaches 2-3, the insulation reaction time is 30-40 minute, pH value is reduced to 6-7, carries out centrifuging after reacting completely, and the gained siccative is put into retort, adding an amount of 5% SILVER REAGENT ammonium chloride solution again in jar stirs, centrifuging is put into retort with siccative and is washed, and washes back oven dry calcination, calcination temperature is about 670 ℃, obtains the high purity vanadic anhydride of purity 〉=99.5%.