CN101987747A - Preparation method of reagent-grade ammonium molybdate - Google Patents
Preparation method of reagent-grade ammonium molybdate Download PDFInfo
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- CN101987747A CN101987747A CN2009103052242A CN200910305224A CN101987747A CN 101987747 A CN101987747 A CN 101987747A CN 2009103052242 A CN2009103052242 A CN 2009103052242A CN 200910305224 A CN200910305224 A CN 200910305224A CN 101987747 A CN101987747 A CN 101987747A
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Abstract
This invention belongs to a preparation method of reagent-grade ammonium molybdate, which comprises the following steps of: (1) feeding, namely adding pure water and 25 percent ammonia water into a reaction pot; raising the temperature to 65 to 75 DEG C; adding industrial molybdate salts with stirring; continuously keeping the temperature when the ratio is 1.3; controlling a pH value to be between 6.2 and 6.6 to totally dissolve the raw materials; stopping feeding materials when the ratio is between 1.42 and 1.45; and preserving the heat and reacting for 0.5 to 1 hour; (2) filtering, namely paving filter cloth, filter paper and treated active carbon in a heat-preserving funnel sequentially; and adding the solution obtained in the step (1) in a vacuumized state into the funnel for filtration; (3) cooling and crystallizing; (4) drying, namely drying the cooled crystal until mother liquor is fully dehydrated; and airing the cooled crystal at normal temperature for a half of a day to obtain the reagent-grade ammonium molybdate. The preparation method of the reagent-grade ammonium molybdate has the advantages of simple process steps, high production efficiency, recycled mother liquor, and no three wastes in the production process.
Description
Technical field
The invention belongs to the chemical reagent field, especially a kind of preparation method of SILVER REAGENT ammonium molybdate.
Background technology
Ammonium molybdate is colourless or little bluish crystallization, can be used for fields such as metallurgy, chemical industry, electronics, analytical chemistry, also can make catalyzer.It is an important reagent of measuring phosphorus, for producing the best materials of acrylonitrile catalyst, also can be used for the production of trace element fertilizer and metal molybdenum.The ammonification purifying that is made as industrial molybdenum salt of reagent ammonium molybdate.Because primary industry molybdenum salt is four molybdenum salt is that [molecular formula is (NH to ammonium tetramolybdate
4)
2Mo
4O
L32H
2O], and finished product SILVER REAGENT ammonium molybdate is that [molecular formula is (NH to seven molybdenum salt
4)
6Mo
7O
244H
2O], thereby in purge process, to add ammoniacal liquor, make to be reflected in the alkali and carry out, do not reach concentration requirement when then dissolving and separate out crystallization but ammonification is excessive; Ammonia residual inadequately then raw material do not dissolve, also do not reach the proportion requirement, so technology is very loaded down with trivial details, production efficiency is lower.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of processing step simple, production efficiency is higher, the mother liquor preparation method who utilizes, do not have in process of production the SILVER REAGENT ammonium molybdate of three wastes generation more capable of circulation.
The present invention is achieved through the following technical solutions:
A kind of preparation method of SILVER REAGENT ammonium molybdate the steps include:
(1), feeds intake: in retort, add pure water and 25% ammoniacal liquor, be warming up to 65-75 ℃, under agitation add industrial molybdenum salt, when proportion reaches 1.3, continue to keep temperature, the control pH value is at 6.2-6.6, raw material is dissolved fully, proportion stops to feed in raw material when 1.42-1.45, insulation reaction 0.5-1 hour, obtains solution A;
(2), filter: the gac of in hot funnel, completing filter cloth, filter paper from down to up and handling well successively, under the state of vacuumizing, in funnel, add the solution A that obtains in the step (1) and filter, cross till the filtrate clear always;
(3), crystallisation by cooling: the solution A after filtering in the step (2) poured in the stainless steel cask of cleaning with distilled water stir the cooling of a bucket external application tap water;
(4), dry: with the refrigerative crystallization put into drier dry purify to mother liquor till, again airing at normal temperatures half a day, can obtain the SILVER REAGENT ammonium molybdate.
And the material mol ratio of described industrial molybdenum salt and ammoniacal liquor is 7: 10.
And described industrial molybdenum salt is ammonium tetramolybdate.
Advantage of the present invention and beneficial effect are:
1, the preparation method of this SILVER REAGENT ammonium molybdate will obtain SILVER REAGENT ammonium molybdate finished product after the dissolving in basic solution of industrial molybdenum salt, filtration, crystallisation by cooling, the drying, this method can fine control ammoniacal liquor addition, make production technique easier, and environment friendly and pollution-free.
2, processing step of the present invention is simple, and production efficiency is higher, the mother liquor preparation method who utilizes, do not have in process of production the SILVER REAGENT ammonium molybdate of three wastes generation more capable of circulation.
Embodiment
The present invention is described in further detail by following examples.Need to prove: following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
Embodiment 1
A kind of preparation method of SILVER REAGENT ammonium molybdate the steps include:
(1), feeds intake: in the 50L retort, add 30L pure water and 10L25% ammoniacal liquor, be warming up to 70 ℃, under agitation industrial ammonium molybdate is slowly added, slow down feed rate after proportion reaches 1.3, continue to keep 70 ℃, the control pH value is 6.3, raw material is dissolved fully, proportion stopped the processing industry ammonium molybdate at 1.44 o'clock, insulation reaction 1 hour obtains solution A;
(2), filter: the gac of in hot funnel, completing filter cloth, filter paper from down to up and handling well successively, under the state of vacuumizing, in funnel, add the solution A that obtains in the step (1) and filter, cross till the filtrate clear always;
(3), crystallisation by cooling: the solution A after filtering in the step (2) is poured in the stainless steel cask of cleaning with distilled water, and not timing is stirred, and makes that crystallization is not lumpd, wall built-up not, the cooling of a bucket external application tap water;
(4), dry: with the refrigerative crystallization put into drier dry purify to mother liquor till, again airing at normal temperatures half a day, can obtain the SILVER REAGENT ammonium molybdate.
Embodiment 2
A kind of preparation method of SILVER REAGENT ammonium molybdate the steps include:
(1), feeds intake: in the 50L retort, add 30L pure water and 10L25% ammoniacal liquor, be warming up to 72 ℃, under agitation industrial ammonium molybdate is slowly added, slow down feed rate after proportion reaches 1.3, continue to keep 72 ℃, the control pH value is 6.5, raw material is dissolved fully, proportion stopped the processing industry ammonium molybdate at 1.42 o'clock, insulation reaction 1 hour obtains solution A;
(2), filter: the gac of in hot funnel, completing filter cloth, filter paper from down to up and handling well successively, under the state of vacuumizing, in funnel, add the solution A that obtains in the step (1) and filter, cross till the filtrate clear always;
(3), crystallisation by cooling: the solution A after filtering in the step (2) is poured in the stainless steel cask of cleaning with distilled water, and not timing is stirred, and makes that crystallization is not lumpd, wall built-up not, the cooling of a bucket external application tap water;
(4), dry: with the refrigerative crystallization put into drier dry purify to mother liquor till, again airing at normal temperatures half a day, can obtain the SILVER REAGENT ammonium molybdate.
Embodiment 3
A kind of preparation method of SILVER REAGENT ammonium molybdate the steps include:
(1), feeds intake: in the 50L retort, add 30L pure water and 10L25% ammoniacal liquor, be warming up to 65 ℃, under agitation industrial ammonium molybdate is slowly added, slow down feed rate after proportion reaches 1.3, continue to keep 65 ℃, the control pH value is 6.5, raw material is dissolved fully, proportion stopped the processing industry ammonium molybdate at 1.45 o'clock, insulation reaction 40 minutes obtains solution A;
(2), filter: the gac of in hot funnel, completing filter cloth, filter paper from down to up and handling well successively, under the state of vacuumizing, in funnel, add the solution A that obtains in the step (1) and filter, cross till the filtrate clear always;
(3), crystallisation by cooling: the solution A after filtering in the step (2) is poured in the stainless steel cask of cleaning with distilled water, and not timing is stirred, and makes that crystallization is not lumpd, wall built-up not, the cooling of a bucket external application tap water;
(4), dry: with the refrigerative crystallization put into drier dry purify to mother liquor till, again airing at normal temperatures half a day, can obtain the SILVER REAGENT ammonium molybdate.
Claims (3)
1. the preparation method of a SILVER REAGENT ammonium molybdate, it is characterized in that: the step of this method of purification is:
(1), feeds intake: in retort, add pure water and 25% ammoniacal liquor, be warming up to 65-75 ℃, under agitation add industrial molybdenum salt, when proportion reaches 1.3, continue to keep temperature, the control pH value is at 6.2-6.6, raw material is dissolved fully, proportion stops to feed in raw material when 1.42-1.45, insulation reaction 0.5-1 hour, obtains solution A;
(2), filter: the gac of in hot funnel, completing filter cloth, filter paper from down to up and handling well successively, under the state of vacuumizing, in funnel, add the solution A that obtains in the step (1) and filter, cross till the filtrate clear always;
(3), crystallisation by cooling: the solution A after filtering in the step (2) poured in the stainless steel cask of cleaning with distilled water stir the cooling of a bucket external application tap water;
(4), dry: with the refrigerative crystallization put into drier dry purify to mother liquor till, again airing at normal temperatures half a day, can obtain the SILVER REAGENT ammonium molybdate.
2. the preparation method of SILVER REAGENT ammonium molybdate according to claim 1 is characterized in that: the material mol ratio of described industrial molybdenum salt and ammoniacal liquor is 7: 10.
3. the preparation method of SILVER REAGENT ammonium molybdate according to claim 1 and 2 is characterized in that: described industrial molybdenum salt is ammonium tetramolybdate.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009103052242A CN101987747A (en) | 2009-08-05 | 2009-08-05 | Preparation method of reagent-grade ammonium molybdate |
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102259927A (en) * | 2011-06-27 | 2011-11-30 | 西部鑫兴金属材料有限公司 | Method for preparing high-purity ammonium tetramolybdate |
| CN103041640A (en) * | 2012-12-28 | 2013-04-17 | 江西稀有稀土金属钨业集团有限公司 | Suction filtration device and filtering method thereof |
| CN105439201A (en) * | 2014-09-30 | 2016-03-30 | 泰州市贝斯特钼制品有限公司 | Method for improving crystal quality of ammonium molybdate |
| CN106986384A (en) * | 2017-06-07 | 2017-07-28 | 中南大学 | A kind of preparation method of ammonium tetramolybdate |
-
2009
- 2009-08-05 CN CN2009103052242A patent/CN101987747A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102259927A (en) * | 2011-06-27 | 2011-11-30 | 西部鑫兴金属材料有限公司 | Method for preparing high-purity ammonium tetramolybdate |
| CN102259927B (en) * | 2011-06-27 | 2012-04-18 | 西部鑫兴金属材料有限公司 | Method for preparing high-purity ammonium tetramolybdate |
| CN103041640A (en) * | 2012-12-28 | 2013-04-17 | 江西稀有稀土金属钨业集团有限公司 | Suction filtration device and filtering method thereof |
| CN105439201A (en) * | 2014-09-30 | 2016-03-30 | 泰州市贝斯特钼制品有限公司 | Method for improving crystal quality of ammonium molybdate |
| CN106986384A (en) * | 2017-06-07 | 2017-07-28 | 中南大学 | A kind of preparation method of ammonium tetramolybdate |
| CN106986384B (en) * | 2017-06-07 | 2018-09-14 | 中南大学 | A kind of preparation method of ammonium tetramolybdate |
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Application publication date: 20110323 |