CN102336427A - Method for preparing electronic grade fine-crystalline barium fluoride - Google Patents
Method for preparing electronic grade fine-crystalline barium fluoride Download PDFInfo
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- CN102336427A CN102336427A CN2011102639143A CN201110263914A CN102336427A CN 102336427 A CN102336427 A CN 102336427A CN 2011102639143 A CN2011102639143 A CN 2011102639143A CN 201110263914 A CN201110263914 A CN 201110263914A CN 102336427 A CN102336427 A CN 102336427A
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Abstract
The invention discloses a method for preparing electronic grade fine-crystalline barium fluoride, which comprises the following steps of: (1), respectively adding barium chloride and water in a reaction vessel, measuring the ion content of non-ferrous metal with an emission spectrometer, and adding carbonate for synthesizing barium carbonate after the ion content is measured to be qualified; (2) adding water and hydrofluoric acid with a ration by weight of 1-3:0.8-1.2 in a reactor, adding the barium carbonate, and agitating 30-60 minutes; (3), heating the reactor until boiling at a temperature of 100-110 DEG C for 15-25 minutes; (4), discharging out of the reactor, and centrifugally separating in a centrifugal device when a pH value is smaller than 0; and (5), drying at a temperature of 200-300 DEG C for 3-5 hours. The method for preparing electronic grade fine-crystalline barium fluoride has the advantages of high product purity capable of reaching more than 5N grade, simple production process, low impurity content, low production cost, capability of massive production and the like.
Description
Technical field
The present invention relates to a kind of preparation method of fine crystallization electronic-grade barium fluoride.
Background technology
China national defence factory proposed to produce fluorophosphate optical glass before 10 years, because it combines the advantage of fluoride glass and phosphate glass, range of application is extremely wide; Have low chromatic dispersion and infrared preferably, ultraviolet perviousness; It is had been widely used in optics, be more suitable for gain medium material simultaneously, can obtain excellent in chemical and mechanical property through the adjustment of making up as high-energy laser; Simultaneously can keep its low phonon energy characteristic, can also be as changing luminous material.
Barium fluoride is one of starting material of producing fluorophosphate optical glass, and the quality of barium fluoride and purity directly influence the quality of fluorophosphate optical glass, at present, produces in the process of barium fluoride; Generate the brilliant barium fluoride of megacryst burl very soon, its density is bigger, precipitate and separate soon after the crystallization; Its nonferrous metal ion content surpasses 5PPM, and it is lower to have the barium fluoride product purity, and production technique is numerous and diverse; Foreign matter content is higher, and the megacryst burl is brilliant, shortcoming such as not can manufacture.
Summary of the invention
The object of the invention promptly is to overcome the deficiency of prior art, provides a kind of product purity to reach more than the 5N level, and production process is simple, and foreign matter content is lower, fine crystallization, the preparation method of a kind of fine crystallization electronic-grade barium fluoride that can manufacture.
The objective of the invention is to realize through following technical scheme: the preparation method of fine crystallization electronic-grade barium fluoride, it may further comprise the steps:
(1) in reaction vessel, adding weight ratio is the bariumchloride and the water of 0.8～1.2:1～3; After the dissolving, measure nonferrous metal ion content with emission spectrometer, when iron ion content wherein less than 0.5PPM; Strontium ion and calcium ion content are during all less than 0.05PPM; Add carbonate again, the carbonate of adding and the weight ratio of bariumchloride are 1～2:0.8～1.2, carbonate synthesis barium;
(2) under the normal temperature, in reaction kettle, adding weight ratio is the water and the hydrofluoric acid of 1～3:0.8～1.2, adds the starchy barium carbonate of water furnishing again, and the barium carbonate of adding and the weight ratio of hydrofluoric acid are 1～1.5:0.6～1, stir 30～60 minutes;
(3) stir to accomplish after, with reaction kettle heated and boiled to 100～110 ℃, the heated and boiled time is 15～25 minutes, its acidity of control is 1～3N in the heated and boiled process;
(4) heated and boiled is accomplished the back and from reaction kettle, is emitted, when its pH value less than 0 the time, automatic spinning in centrifugal device;
(5) oven dry is handled, and bake out temperature is 200～300 ℃, and drying time is 3～5 hours, obtains the electronic-grade barium fluoride.The invention has the beneficial effects as follows: the present invention provides a kind of preparation method of fine crystallization electronic-grade barium fluoride; Adopt the fine crystallization mode, its nonferrous metal ion content has product purity and reaches more than the 5N level less than 0.5PPM; Production process is simple; Foreign matter content is lower, and production cost is low, advantage such as can produce in batches.
Embodiment
Below in conjunction with embodiment the present invention is done further description, but protection scope of the present invention is not limited to the following stated.
Embodiment 1:
The preparation method of fine crystallization electronic-grade barium fluoride, it may further comprise the steps:
(1) in reaction vessel, adding weight ratio is bariumchloride and the water of 0.8:1; After the dissolving, measure nonferrous metal ion content with emission spectrometer, when iron ion content wherein less than 0.5PPM; Strontium ion and calcium ion content are during all less than 0.05PPM; Add carbonate again, the carbonate of adding and the weight ratio of bariumchloride are 1:0.8, carbonate synthesis barium;
(2) under the normal temperature, in reaction kettle, adding weight ratio is water and the hydrofluoric acid of 1:0.8, adds the starchy barium carbonate of water furnishing again, and the barium carbonate of adding and the weight ratio of hydrofluoric acid are 1:0.6, stir 30 minutes;
(3) stir to accomplish after, with reaction kettle heated and boiled to 110 ℃, the heated and boiled time is 25 minutes, its acidity of control is 1N in the heated and boiled process;
(4) heated and boiled is accomplished the back and from reaction kettle, is emitted, when its pH value less than 0 the time, automatic spinning in centrifugal device;
(5) oven dry is handled, and bake out temperature is 200 ℃, and drying time is 3 hours, obtains the electronic-grade barium fluoride.
Embodiment 2:
The preparation method of fine crystallization electronic-grade barium fluoride, it may further comprise the steps:
(1) in reaction vessel, adding weight ratio is bariumchloride and the water of 1.2:3; After the dissolving, measure nonferrous metal ion content with emission spectrometer, when iron ion content wherein less than 0.5PPM; Strontium ion and calcium ion content are during all less than 0.05PPM; Add carbonate again, the carbonate of adding and the weight ratio of bariumchloride are 2:1.2, carbonate synthesis barium;
(2) under the normal temperature, in reaction kettle, adding weight ratio is water and the hydrofluoric acid of 3:1.2, adds the starchy barium carbonate of water furnishing again, and the barium carbonate of adding and the weight ratio of hydrofluoric acid are 1.5:1, stir 60 minutes;
(3) stir to accomplish after, with reaction kettle heated and boiled to 100 ℃, the heated and boiled time is 15 minutes, its acidity of control is 3N in the heated and boiled process;
(4) heated and boiled is accomplished the back and from reaction kettle, is emitted, when its pH value less than 0 the time, automatic spinning in centrifugal device;
(5) oven dry is handled, and bake out temperature is 300 ℃, and drying time is 5 hours, obtains the electronic-grade barium fluoride.
Embodiment 3:
The preparation method of fine crystallization electronic-grade barium fluoride, it may further comprise the steps:
(1) in reaction vessel, adding weight ratio is bariumchloride and the water of 1:2; After the dissolving, measure nonferrous metal ion content with emission spectrometer, when iron ion content wherein less than 0.5PPM; Strontium ion and calcium ion content are during all less than 0.05PPM; Add carbonate again, the carbonate of adding and the weight ratio of bariumchloride are 1.5:1, carbonate synthesis barium;
(2) under the normal temperature, in reaction kettle, adding weight ratio is water and the hydrofluoric acid of 2:1, adds the starchy barium carbonate of water furnishing again, and the barium carbonate of adding and the weight ratio of hydrofluoric acid are 1.2:0.8, stir 45 minutes;
(3) stir to accomplish after, with reaction kettle heated and boiled to 105 ℃, the heated and boiled time is 20 minutes, its acidity of control is 2N in the heated and boiled process;
(4) heated and boiled is accomplished the back and from reaction kettle, is emitted, when its pH value less than 0 the time, automatic spinning in centrifugal device;
(5) oven dry is handled, and bake out temperature is 250 ℃, and drying time is 4 hours, obtains the electronic-grade barium fluoride.
Claims (1)
1. the preparation method of fine crystallization electronic-grade barium fluoride, it is characterized in that: it may further comprise the steps:
(1) in reaction vessel, adding weight ratio is the bariumchloride and the water of 0.8～1.2:1～3; After the dissolving, measure nonferrous metal ion content with emission spectrometer, when iron ion content wherein less than 0.5PPM; Strontium ion and calcium ion content are during all less than 0.05PPM; Add carbonate again, the carbonate of adding and the weight ratio of bariumchloride are 1～2:0.8～1.2, carbonate synthesis barium;
(2) under the normal temperature, in reaction kettle, adding weight ratio is the water and the hydrofluoric acid of 1～3:0.8～1.2, adds the starchy barium carbonate of water furnishing again, and the barium carbonate of adding and the weight ratio of hydrofluoric acid are 1～1.5:0.6～1, stir 30～60 minutes;
(3) stir to accomplish after, with reaction kettle heated and boiled to 100～110 ℃, the heated and boiled time is 15～25 minutes, its acidity of control is 1～3N in the heated and boiled process;
(4) heated and boiled is accomplished the back and from reaction kettle, is emitted, when its pH value less than 0 the time, automatic spinning in centrifugal device;
(5) oven dry is handled, and bake out temperature is 200～300 ℃, and drying time is 3～5 hours, obtains the electronic-grade barium fluoride.
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| CN2011102639143A CN102336427A (en) | 2011-09-07 | 2011-09-07 | Method for preparing electronic grade fine-crystalline barium fluoride |
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| CN2011102639143A CN102336427A (en) | 2011-09-07 | 2011-09-07 | Method for preparing electronic grade fine-crystalline barium fluoride |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104849165A (en) * | 2015-05-14 | 2015-08-19 | 湖北新华光信息材料有限公司 | Test method of content of high-purity barium fluoride |
| CN113233491A (en) * | 2021-05-12 | 2021-08-10 | 江西渠成氟化学有限公司 | Impurity removal method for calcium fluoride |
| CN113247937A (en) * | 2021-05-12 | 2021-08-13 | 江西渠成氟化学有限公司 | Impurity removal method for barium fluoride |
| CN113998725A (en) * | 2021-11-30 | 2022-02-01 | 贵州红星发展股份有限公司 | Barium fluoride and preparation method thereof |
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| US4053572A (en) * | 1976-05-17 | 1977-10-11 | The Harshaw Chemical Company | Process for preparing essentially pure barium fluoride crystals |
| RU1778071C (en) * | 1990-12-04 | 1992-11-30 | Специальное Конструкторско-Технологическое Бюро Ан Таджсср | Method for producing barium fluoride |
| CN101376519A (en) * | 2007-08-31 | 2009-03-04 | 多氟多化工股份有限公司 | Method for preparing barium fluoride |
| CN101676213A (en) * | 2008-09-16 | 2010-03-24 | 多氟多化工股份有限公司 | Method for dry preparation of barium fluorosilicate and barium fluoride |
| CN101967003A (en) * | 2010-10-25 | 2011-02-09 | 宁波诺尔丽化学科技有限公司 | Method for preparing barium fluoride from organic fluoridation waste |
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2011
- 2011-09-07 CN CN2011102639143A patent/CN102336427A/en active Pending
Patent Citations (5)
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| US4053572A (en) * | 1976-05-17 | 1977-10-11 | The Harshaw Chemical Company | Process for preparing essentially pure barium fluoride crystals |
| RU1778071C (en) * | 1990-12-04 | 1992-11-30 | Специальное Конструкторско-Технологическое Бюро Ан Таджсср | Method for producing barium fluoride |
| CN101376519A (en) * | 2007-08-31 | 2009-03-04 | 多氟多化工股份有限公司 | Method for preparing barium fluoride |
| CN101676213A (en) * | 2008-09-16 | 2010-03-24 | 多氟多化工股份有限公司 | Method for dry preparation of barium fluorosilicate and barium fluoride |
| CN101967003A (en) * | 2010-10-25 | 2011-02-09 | 宁波诺尔丽化学科技有限公司 | Method for preparing barium fluoride from organic fluoridation waste |
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| 韩汉民: "高纯氟化钡的制备", 《陕西化工》, no. 1, 31 December 2004 (2004-12-31), pages 20 - 22 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104849165A (en) * | 2015-05-14 | 2015-08-19 | 湖北新华光信息材料有限公司 | Test method of content of high-purity barium fluoride |
| CN113233491A (en) * | 2021-05-12 | 2021-08-10 | 江西渠成氟化学有限公司 | Impurity removal method for calcium fluoride |
| CN113247937A (en) * | 2021-05-12 | 2021-08-13 | 江西渠成氟化学有限公司 | Impurity removal method for barium fluoride |
| CN113998725A (en) * | 2021-11-30 | 2022-02-01 | 贵州红星发展股份有限公司 | Barium fluoride and preparation method thereof |
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Application publication date: 20120201 |