CN103449523A - Preparation method of extracted high-purity molybdenum trioxide - Google Patents

Preparation method of extracted high-purity molybdenum trioxide Download PDF

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Publication number
CN103449523A
CN103449523A CN2012101863767A CN201210186376A CN103449523A CN 103449523 A CN103449523 A CN 103449523A CN 2012101863767 A CN2012101863767 A CN 2012101863767A CN 201210186376 A CN201210186376 A CN 201210186376A CN 103449523 A CN103449523 A CN 103449523A
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CN
China
Prior art keywords
temperature
molybdenum trioxide
furnace
subliming furnace
purity molybdenum
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CN2012101863767A
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Chinese (zh)
Inventor
陈方吾
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湖北中澳纳米材料技术有限公司
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Priority to CN2012101863767A priority Critical patent/CN103449523A/en
Publication of CN103449523A publication Critical patent/CN103449523A/en

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    • Y02P20/124

Abstract

The invention relates to the field of molybdenum trioxide, and specifically relates to a preparation method of extracted high-purity molybdenum trioxide. The preparation method is characterized by comprising the following steps: treating industrial molybdic acid to remove moisture, oil and various trace impurities with a volatilization point lower than 750 DEG C in materials; metering according to sublimation speed for feeding the materials into a subliming furnace, and controlling the temperature of the subliming furnace to 1100 DEG C-1160 DEG C; selectively adopting clean air coiling or liquid nitrogen cooling according to the requirements of the grain size, and controlling the temperature to 250 DEG C or 50 DEG C; collecting the dust by a primary metal membrane for recycling with a yield of 99%, and collecting the dust by a secondary cloth bag with the yield of 1% to recycle high-purity molybdenum trioxide. The technical scheme is adopted, and the subliming furnace is used as a carbon rod for directly heating up, and therefore, the heating efficiency is high, the temperature is controlled by using a computer, and a temperature fluctuation range is +/-1 DEG C. Residues at the furnace bottom are calculated according to material balance and exhausted regularly, and waste of the residues is used as steel-making ferro-molybdenum after being cooled or used as the material for producing sodium molybdate after being crushed. The preparation method disclosed by the invention is safe and reliable in process, high in recovery rate and high in quality, thereby improving production efficiency and relieving labor intensity of operation personnel.

Description

A kind of preparation method who extracts high-purity molybdenum trioxide

Technical field

The present invention relates to the molybdic oxide field, is a kind of preparation method who extracts high-purity molybdenum trioxide.

Background technology

Generally the method for application is now: will make the elaboration ammonium molybdate containing the raw material of molybdenum, the refining ammonium molybdate of heating generates high-purity molybdenum trioxide.Ammonium molybdate is made through roasting, lixiviate, removal of impurities, the techniques such as concentrated, acid is heavy, filtration by the above concentrated molybdenum ore of molybdenum content 40%, yield 95% left and right of molybdenum.Therefore give birth to waste gas in process, waste water, waste residue amount large, the environmental protection difficulty is large,, expense is high.

Summary of the invention

The objective of the invention is to propose a kind of technique simple, consuming time short, energy consumption is low, quality good, the preparation method of eco-friendly processing high purity molybdic oxide.

Technical scheme of the present invention is: it is characterized in that industrial molybdic acid is after processing, remove moisture content, oil and volatilization point in material at the various trace impurities below 750 ℃; According to rate of sublimation, metering feeds subliming furnace by material, and the subliming furnace temperature is controlled at 1100~1160 ℃; Or cooled with liquid nitrogen cooling with uncontaminated air are selected in requirement to granularity, and temperature is controlled at 250 ℃ or 50 ℃; The recovery of gathering dust of one-level metallic membrane, yield is 99%, secondary bag collection 1% reclaims high-purity molybdenum trioxide.

Owing to having taked technique scheme, the use subliming furnace is the carbon-point direct heating, so thermo-efficiency is high, and temperature control is controlled with computer, temperature fluctuation range ± 1 ℃.The furnace bottom residue calculates according to material balance, regularly discharge, the cooling rear work steel-making molybdenum-iron of its waste material or the rear raw material of making to produce Sodium orthomolybdate of pulverizing.This process safety is reliable, the rate of recovery is high, environmental friendliness, be convenient to automatization control, technique simple, consuming time short, energy consumption is low, quality is high, has improved production efficiency, has alleviated operator's labour intensity.

Embodiment

Below in conjunction with embodiment, the present invention is further illustrated.

Embodiment 1

1, industrial molybdic acid gives processing.750 ℃ for the treatment of temps, remove moisture and oil in material, and remove that in material, volatilization point is at other trace impurity below 750 ℃, and the material molybdic oxide content after processing is more than 98%; Impurity to material accurately detects;

2, according to rate of sublimation, metering is sent material into subliming furnace, if containing metal calcium constituent in material, the subliming furnace Control for Kiln Temperature is at 1100 ℃.

3, select the cooling or cooled with liquid nitrogen of uncontaminated air according to customer requirements, the one-level temperature before retrieving arrangement of gathering dust is controlled at 250 ℃ or 50 ℃;

4, reclaim through the I and II gas solid separation, collect product (nano level) high-purity molybdenum trioxide;

5, the subliming furnace residue calculates according to material balance, regularly discharge.

Embodiment 2

1, industrial molybdic acid gives processing.750 ℃ for the treatment of temps, remove moisture and oil in material, and remove that in material, volatilization point is at other trace impurity below 750 ℃, and the material molybdic oxide content after processing is more than 98%; Impurity to material accurately detects;

According to rate of sublimation metering, material is sent into to subliming furnace, if containing metal calcium constituent not in material, the subliming furnace Control for Kiln Temperature is at 1160 ℃.

2, select the cooling or cooled with liquid nitrogen of uncontaminated air according to customer requirements, the one-level temperature before retrieving arrangement of gathering dust is controlled at 250 ℃ or 50 ℃;

3, reclaim through the I and II gas solid separation, collect product (nano level) high-purity molybdenum trioxide;

4, the subliming furnace residue calculates according to material balance, regularly discharge.

Claims (1)

1. a preparation method who extracts high-purity molybdenum trioxide, is characterized in that industrial molybdic acid is after processing, removes moisture content, oil and volatilization point in material at the various trace impurities below 750 ℃; According to rate of sublimation, metering feeds subliming furnace by material, and the subliming furnace temperature is controlled at 1100~1160 ℃; Or cooled with liquid nitrogen cooling with uncontaminated air are selected in requirement to granularity, and temperature is controlled at 250 ℃ or 50 ℃; The recovery of gathering dust of one-level metallic membrane, yield is 99%, secondary bag collection 1% reclaims high-purity molybdenum trioxide.
CN2012101863767A 2012-06-04 2012-06-04 Preparation method of extracted high-purity molybdenum trioxide CN103449523A (en)

Priority Applications (1)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103818960A (en) * 2014-03-03 2014-05-28 浙江理工大学 Method for preparing alpha-MoO3 nanobelt by adopting hot-wire chemical vapor deposition technology
CN105329945A (en) * 2015-12-04 2016-02-17 湖北中澳纳米材料技术有限公司 Device and method for preparing high-purity and high-dissolvability molybdenum trioxide with industrial molybdic acid
WO2017092712A1 (en) * 2015-12-04 2017-06-08 湖北中澳纳米材料技术有限公司 Device and method for producing high-purity nano molybdenum trioxide
CN107381642A (en) * 2017-09-19 2017-11-24 芜湖人本合金有限责任公司 High-purity molybdenum trioxide and preparation method thereof
CN107522231A (en) * 2017-09-19 2017-12-29 芜湖人本合金有限责任公司 High-purity molybdenum trioxide and preparation method thereof
CN108193060A (en) * 2018-01-04 2018-06-22 中南大学 The method of rhenium-containing molybdenum concntrate volatilization-water logging separation molybdenum-rhenium

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6468497B1 (en) * 2000-11-09 2002-10-22 Cyprus Amax Minerals Company Method for producing nano-particles of molybdenum oxide

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6468497B1 (en) * 2000-11-09 2002-10-22 Cyprus Amax Minerals Company Method for producing nano-particles of molybdenum oxide

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103818960A (en) * 2014-03-03 2014-05-28 浙江理工大学 Method for preparing alpha-MoO3 nanobelt by adopting hot-wire chemical vapor deposition technology
CN103818960B (en) * 2014-03-03 2015-06-17 浙江理工大学 Method for preparing alpha-MoO3 nanobelt by adopting hot-wire chemical vapor deposition technology
CN105329945A (en) * 2015-12-04 2016-02-17 湖北中澳纳米材料技术有限公司 Device and method for preparing high-purity and high-dissolvability molybdenum trioxide with industrial molybdic acid
WO2017092712A1 (en) * 2015-12-04 2017-06-08 湖北中澳纳米材料技术有限公司 Device and method for producing high-purity nano molybdenum trioxide
GB2559305A (en) * 2015-12-04 2018-08-01 Hubei Zhongao Nanotech Co Ltd Device and method for producing high-purity nano molybdenum trioxide
US10745290B2 (en) 2015-12-04 2020-08-18 Hubei Zhong'ao Nanotech Co., Ltd Device and method for producing high-purity nano molybdenum trioxide
CN107381642A (en) * 2017-09-19 2017-11-24 芜湖人本合金有限责任公司 High-purity molybdenum trioxide and preparation method thereof
CN107522231A (en) * 2017-09-19 2017-12-29 芜湖人本合金有限责任公司 High-purity molybdenum trioxide and preparation method thereof
CN108193060A (en) * 2018-01-04 2018-06-22 中南大学 The method of rhenium-containing molybdenum concntrate volatilization-water logging separation molybdenum-rhenium

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Application publication date: 20131218