CN103601208B - The preparation method of micro-nano structure boron calcium composite oxides - Google Patents
The preparation method of micro-nano structure boron calcium composite oxides Download PDFInfo
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- CN103601208B CN103601208B CN201310603617.8A CN201310603617A CN103601208B CN 103601208 B CN103601208 B CN 103601208B CN 201310603617 A CN201310603617 A CN 201310603617A CN 103601208 B CN103601208 B CN 103601208B
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- composite oxides
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- boric acid
- boron calcium
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Abstract
The invention discloses a kind of preparation method of micro-nano structure boron calcium composite oxides.First water, boric acid are joined in reaction vessel respectively and dissolve, after temperature is raised to 30 ~ 80 DEG C, add unslaked lime or white lime, after turbulent flow circulates 60 ~ 240 minutes, filtering separation; Filter cake was in 80 ~ 120 DEG C of dryings 1 ~ 10 hour, and in said process, boric acid is the quality 3 ~ 3.5 times of unslaked lime, or is 1.5 ~ 2.5 times of white lime quality.The method prepares the knitting wool bulk boron calcium composite oxides nanometer sheet cluster of good fluidity, polymolecularity, primary particle is less than 100nm, clustered particles size is between 5 ~ 10 μm, and this product can be used for the fire retardant of polymkeric substance, and inorganic composite materials strengthens, rapid solidification agent.
Description
Technical field
The present invention relates to a kind of preparation method with the boron calcium composite oxides of micro-nano structure, belong to technical field of inorganic material.
Background technology
Boron calcium composite oxides are widely used in industrial goods processing, the productions such as pharmacy, building coating, pigment, pottery, glass, papermaking, rubber and plastics.
Micro nano structure boron calcium composite oxides, because of its efficient dispersed and mobility, can improve the processing characteristics of matrix material better, and effectively can improve the mechanical property of material.
The present invention adopts the disposable synthesis in enormous quantities of turbulent circulating technology to have boron calcium composite oxides nano-sheet cluster (knitting wool bulk) of micro-nano structure, and this product can be used as the fire retardant of superpolymer, the enhancing of matrix material, rapid solidification agent.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of boron calcium CaO1.5B with micro-nano structure
2o
3h
2the preparation method of O composite oxides.The method mild condition, technological process is simple, products obtained therefrom good fluidity, good dispersity.
Technical scheme of the present invention is:
First water, boric acid are joined in reaction vessel respectively and dissolve, after temperature is raised to 30 ~ 80 DEG C, add unslaked lime or white lime, after turbulent flow circulates 60 ~ 240 minutes, filtering separation; Filter cake was in 80 ~ 120 DEG C of dryings 1 ~ 10 hour, and in said process, boric acid is the quality 3 ~ 3.5 times of unslaked lime, or is 1.5 ~ 2.5 times of white lime quality.The quality of water used is 1.0 ~ 3.0 times of boric acid quality.
The inventive method prepares the knitting wool bulk boron calcium composite oxides nanocluster of good fluidity, polymolecularity, primary particle is less than 100nm, clustered particles size is between 5 ~ 10 μm, and this product can be used for the fire retardant of polymkeric substance, inorganic composite materials rapid solidification agent.
Accompanying drawing explanation
Fig. 1 embodiment 1 obtain boron calcium composite oxides nanocluster SEM figure.
Embodiment
Embodiment 1:
Measure 100 water and 80 grams of boric acid respectively, join in reactor, warming while stirring is to 30 DEG C, add 28 grams of unslaked limes again, be warming up to 80 DEG C, turbulent flow circulation is after 200 minutes, direct filtration, filtrate recovery is directly used in preparation next time use, and filter cake directly obtains product in 1 hour in 120 DEG C of dryings.
Embodiment 2:
Measure 160 water and 80 grams of boric acid respectively, join in reactor, warming while stirring is to 50 DEG C, add 36 grams of white limes again, be warming up to 70 DEG C, turbulent flow circulation is after 60 minutes, direct filtration, filtrate recovery is directly used in preparation next time use, and filter cake directly obtains product in 3 hours in 100 DEG C of dryings.
Embodiment 3:
Measure 200 water and 80 grams of boric acid respectively, join in reactor, warming while stirring is to 30 DEG C, add 42 grams of white limes again, be warming up to 40 DEG C, turbulent flow circulation is after 240 minutes, direct filtration, filtrate recovery is directly used in preparation next time use, and filter cake directly obtains product in 10 hours in 80 DEG C of dryings.
Claims (3)
1. a preparation method for micro-nano structure boron calcium composite oxides, is characterized in that, first water, boric acid is joined in reaction vessel respectively and dissolves, after temperature is raised to 30 ~ 80 DEG C, add unslaked lime or white lime, after turbulent flow circulates 60 ~ 240 minutes, and filtering separation; Filter cake was in 80 ~ 120 DEG C of dryings 1 ~ 10 hour, and in said process, boric acid is 3 ~ 3.5 times of Lime Quality, or is 1.5 ~ 2.5 times of white lime quality.
2. preparation method as claimed in claim 1, is characterized in that: the quality of water is 1.2 ~ 2.0 times of boric acid quality.
3. preparation method as claimed in claim 1 or 2, is characterized in that: obtained boron calcium composite oxides nanocluster, primary particle thickness direction is less than 100nm, and clustered particles size is between 5 ~ 10 μm.
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| CN201310603617.8A CN103601208B (en) | 2013-11-25 | 2013-11-25 | The preparation method of micro-nano structure boron calcium composite oxides |
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| CN201310603617.8A CN103601208B (en) | 2013-11-25 | 2013-11-25 | The preparation method of micro-nano structure boron calcium composite oxides |
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| CN103601208A CN103601208A (en) | 2014-02-26 |
| CN103601208B true CN103601208B (en) | 2015-11-18 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103922391A (en) * | 2014-04-29 | 2014-07-16 | 武汉大学 | Preparation method of boron zinc composite oxide in micronano structure |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56120513A (en) * | 1980-02-22 | 1981-09-21 | Agency Of Ind Science & Technol | Manufacture of calcium borate |
| SU948882A1 (en) * | 1980-07-16 | 1982-08-07 | Приморское Ордена "Знак Почета" Производственное Объединение "Бор" Им.50-Летия Ссср | Method for preparing calcium borate |
| SU1144978A1 (en) * | 1983-06-08 | 1985-03-15 | Предприятие П/Я А-7125 | Method of obtaining calcium borate |
| CN1170696A (en) * | 1996-07-11 | 1998-01-21 | 麦特里斯－普莱麦斯－玛格达伦纳公司 | Process for production of purified, synthetic calcium borate |
| US5869014A (en) * | 1995-03-01 | 1999-02-09 | Carranza; Manuel Camarena | Process for the production of purified, synthetic calcium borate |
| CN1252775A (en) * | 1997-04-18 | 2000-05-10 | 美国博拉克有限公司 | Method for producing calcium borate |
-
2013
- 2013-11-25 CN CN201310603617.8A patent/CN103601208B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56120513A (en) * | 1980-02-22 | 1981-09-21 | Agency Of Ind Science & Technol | Manufacture of calcium borate |
| SU948882A1 (en) * | 1980-07-16 | 1982-08-07 | Приморское Ордена "Знак Почета" Производственное Объединение "Бор" Им.50-Летия Ссср | Method for preparing calcium borate |
| SU1144978A1 (en) * | 1983-06-08 | 1985-03-15 | Предприятие П/Я А-7125 | Method of obtaining calcium borate |
| US5869014A (en) * | 1995-03-01 | 1999-02-09 | Carranza; Manuel Camarena | Process for the production of purified, synthetic calcium borate |
| CN1170696A (en) * | 1996-07-11 | 1998-01-21 | 麦特里斯－普莱麦斯－玛格达伦纳公司 | Process for production of purified, synthetic calcium borate |
| CN1252775A (en) * | 1997-04-18 | 2000-05-10 | 美国博拉克有限公司 | Method for producing calcium borate |
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