CN102219261B - Production process of high-sodium WO3 - Google Patents

Abstract

The invention discloses a production process of high-sodium WO3, which comprises the following production steps: preparing a 200 g/L sodium carbonate solution; pre-adjusting the ammonia content in a 250-270 g/L (NH4)2WO4 solution to 50-70 g/L, adding the (NH4)2WO4 solution with adjusted ammonia content to a thermal reaction kettle, carrying out evaporation concentration at the temperature of 50-100 DEG C for volatilizing ammonia till pH is reduced to 7.5-8.4 and baume degree Be is 2 and maintaining air pressure at 0.3 MPa, adding a sodium carbonate solution, wherein the mass ratio of sodium carbonate to (NH4)2WO4 is 1:(21-23), continuing to heat till baume degree Be becomes 1, stopping heating and cooling to 45-55 DEG C; and carrying out solid-liquid separation to obtain an ammonium paratungstate product, then soaking in an ammonium nitrate solution with mass percentage of 5% for 2 hours, draining again, calcining the ammonium paratungstate product in a 730-765 DEG C high-temperature furnace for 40 minutes to obtain high-sodium WO3. The high-sodium WO3 prepared by the production process provided by the invention has the advantages of high purity, complete particle size development, uniform distribution of chemical main components and excellent use performance.

Description

A kind of high sodium WO 3Production technique

Technical field

The present invention relates to tungsten industry field, specifically is a kind of high sodium WO ₃Production technique.

Background technology

Common specification WO ₃Be applicable to and produce the coarse particles tungsten powder, when producing ultra coarse particles tungsten powder, then need improve WO ₃In sodium element content.Ordinary method has spray method, artificial doping method.Spray method is in advance yellow soda ash to be made into certain density solution, is ejected into common specification WO through atomizer ₃The surface obtains high sodium WO through the blender batch mixing then ₃Another kind of artificial doping rule is directly toward WO ₃A certain amount of yellow soda ash of middle adding is used the blender batch mixing then.The defective of these two kinds of methods is the high sodium WO that makes ₃The chemical element skewness influences follow-up production, and it is inhomogeneous to cause particle to be grown up, and the product differentiation of producing is very big.In addition, spray method also need be bought atomizer, causes the increase of cost.

Summary of the invention

For overcoming above-mentioned deficiency, the invention provides a kind of high sodium WO ₃Production technique, to overcome ordinary method WO ₃In sodium element defective pockety, and this method need not to acquire new installation, only needs on original process base, just can carry out, and reduced cost.

Solution of the present invention is in evaporation and crystal process; Under certain pressure, mother-in-law U.S. degree, pH value condition, add the sodium carbonate solution for preparing in advance; Stirring, evaporative crystallization, solid-liquid separation can obtain adsorbing the high ammonium paratungstate goods of sodium content, and the ammonium paratungstate goods are calcined under the open type condition and promptly obtained the high sodium WO that sodium element is evenly distributed ₃

The high sodium WO of the present invention ₃Production technique, comprise following production stage:

(1) compound concentration is that the sodium carbonate solution of 200g/L is subsequent use in advance;

(2) be 250～270g/L (NH to concentration ₄) ₂WO ₄Solution preset ammonia content, control (NH ₄) ₂WO ₄Ammonia concentration in the solution is between 50～70g/L, with (the NH behind the accent ammonia ₄) ₂WO ₄Solution adds in the thermal response still, 50～100 ℃ of following evaporation concentration, ammonia volatilization to pH value is dropped between 7.5～8.4; Mother-in-law U.S. degree ° B é=2; Air pressure remains on 0.3MPa, slowly adds the above-mentioned sodium carbonate solution that configures, the yellow soda ash of adding and (NH while stirring ₄) ₂WO ₄Mass ratio 1: 21～23, continue to be heated to mother-in-law U.S. degree ° B é=1 o'clock, stop heating, be cooled to 45～55 ℃;

(3) filter, wash, calcine: adopt the vacuum filtration mode to carry out solid-liquid separation above-mentioned feed liquid; Promptly obtain the high ammonium paratungstate goods of sodium content absorption; Using mass percent again is that 5% ammonium nitrate solution soaked 2 hours; After draining once more, the ammonium paratungstate goods are placed in 730～765 ℃ of High Temperature Furnaces Heating Apparatuss calcining 40 minutes, promptly obtain the high sodium WO that sodium element is evenly distributed ₃

The high sodium WO that the present invention makes ₃, purity is high, and granularity is grown complete, and chemical main content distribution is even, and use properties is excellent.

Embodiment

Prepare 0.3m in advance ³Concentration is that the sodium carbonate solution of 200g/L is subsequent use;

To volume is 5m ³, concentration is at 260g/L (NH ₄) ₂WO ₄Solution preset ammonia content, control (NH ₄) ₂WO ₄Ammonia concentration in the solution is at 65g/L, with (the NH behind the accent ammonia ₄) ₂WO ₄Solution adds in the thermal response still, 80 ℃ of following evaporation concentration, makes ammonia volatilization drop to 8.0 to the pH value, mother-in-law U.S. degree ° B é=2, and air pressure remains on 0.3MPa, slowly adds the above-mentioned sodium carbonate solution that configures while stirring; Yellow soda ash that adds and (NH ₄) ₂WO ₄Mass ratio be (0.3m ³* 200g/L): (5m ³* 260g/L), between 1: 21～23; Continue to be heated to mother-in-law U.S. degree ° B é=1 o'clock, stop heating, be cooled to 50 ℃;

Adopt the vacuum filtration mode to carry out solid-liquid separation to above-mentioned feed liquid; Promptly obtain the high ammonium paratungstate goods of sodium content absorption; Using mass percent again is that 5% ammonium nitrate solution soaked 2 hours; After draining once more, the ammonium paratungstate goods are placed in 750 ℃ of High Temperature Furnaces Heating Apparatuss calcining 40 minutes, can obtain the high sodium WO that sodium element is evenly distributed ₃

Claims (1)

1. one kind high sodium WO ₃Production technique, it is characterized in that, comprise following production stage:

(1) compound concentration is that the sodium carbonate solution of 200g/L is subsequent use in advance;

(2) be 250-270g/L (NH to concentration ₄) ₂WO ₄Solution preset ammonia content, control (NH ₄) ₂WO ₄Ammonia concentration in the solution is between 50～70g/L, with (the NH behind the accent ammonia ₄) ₂WO ₄Solution adds in the thermal response still, 50～100 ℃ of following evaporation concentration, ammonia volatilization to pH value is dropped between 7.5～8.4; Mother-in-law U.S. degree ° B é=2; Air pressure remains on 0.3MPa, slowly adds the above-mentioned sodium carbonate solution that configures, the yellow soda ash of adding and (NH while stirring ₄) ₂WO ₄Mass ratio 1: 21～23, continue to be heated to mother-in-law U.S. degree ° B é=1 o'clock, stop heating, be cooled to 45～55 ℃;

(3) filter, wash, calcine: adopt the vacuum filtration mode to carry out solid-liquid separation above-mentioned feed liquid; Promptly obtain the high ammonium paratungstate goods of sodium content absorption; Using mass percent again is that 5% ammonium nitrate solution soaked 2 hours; After draining once more, the ammonium paratungstate goods are placed in 730～765 ℃ of High Temperature Furnaces Heating Apparatuss calcining 40 minutes, promptly obtain the high sodium WO that sodium element is evenly distributed ₃