CN103601208A - Preparation method of boron and calcium composite oxide with micro-nano structure - Google Patents
Preparation method of boron and calcium composite oxide with micro-nano structure Download PDFInfo
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- CN103601208A CN103601208A CN201310603617.8A CN201310603617A CN103601208A CN 103601208 A CN103601208 A CN 103601208A CN 201310603617 A CN201310603617 A CN 201310603617A CN 103601208 A CN103601208 A CN 103601208A
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- boric acid
- boron
- calcium composite
- composite oxide
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Abstract
The invention discloses a preparation method of a boron and calcium composite oxide with a micro-nano structure. The preparation method comprises the steps of firstly, respectively adding water and boric acid into a reaction vessel, dissolving the boric acid, adding quick lime or hydrated lime after the temperature is raised to 30-80 DEG C, and filtering and separating after carrying out turbulent flow circulation for 60-240min; drying a filter cake at the temperature of 80-120 DEG C for 1-10h, wherein the mass of the boric acid is 3-3.5 times that of the quick lime or 1.5-2.5 times that of the hydrated lime. The method can be used for preparing a coiling type boron and calcium composite oxide nanosheet cluster with good flowability and high dispersibility, wherein the particle size of a primary particle is smaller than 100nm, and the particle size of a cluster particle ranges from 5mu m to 10mu m. The boron and calcium composite oxide can be used as a flame retardant of a polymer and an agent for enhancing and rapidly coagulating an inorganic composite material.
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 dispersiveness and mobility, can improve the processing characteristics of matrix material better, and can effectively improve the mechanical property of material.
The present invention adopts the disposable boron calcium composite oxides nano-sheet cluster (knitting wool bulk) with micro-nano structure in enormous quantities synthetic of turbulent circulating technology, 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 and dissolved respectively, until temperature, be raised to after 30～80 ℃, add unslaked lime or white lime, after turbulent flow circulates 60～240 minutes, filtering separation; Filter cake in 80～120 ℃ dry 1～10 hour, in said process, 3～3.5 times of quality that boric acid is unslaked lime, or be 1.5～2.5 times of white lime quality.The quality of institute's water is 1.0～3.0 times of boric acid quality.
The inventive method is prepared the knitting wool bulk boron calcium composite oxides nanocluster of good fluidity, polymolecularity, primary particle is less than 100nm, cluster granular size is between 5～10 μ m, and this product can be used for the fire retardant of polymkeric substance, inorganic composite materials rapid solidification agent.
Accompanying drawing explanation
The SEM figure of the resulting boron calcium of Fig. 1 embodiment 1 composite oxides nanocluster.
Embodiment
Embodiment 1:
Measure respectively 100 water and 80 grams of boric acid, join in reactor warming while stirring to 30 ℃, add 28 grams of unslaked limes again, be warming up to 80 ℃, turbulent flow circulation is after 200 minutes, direct filtration, filtrate recovery is directly used in preparation next time use, and filter cake is directly in 120 ℃ of dry products that obtain for 1 hour.
Embodiment 2:
Measure respectively 160 water and 80 grams of boric acid, join in reactor warming while stirring to 50 ℃, add 36 grams of white limes again, be warming up to 70 ℃, turbulent flow circulation is after 60 minutes, direct filtration, filtrate recovery is directly used in preparation next time use, and filter cake is directly in 100 ℃ of dry products that obtain for 3 hours.
Embodiment 3:
Measure respectively 200 water and 80 grams of boric acid, join in reactor warming while stirring to 30 ℃, add 42 grams of white limes again, be warming up to 40 ℃, turbulent flow circulation is after 240 minutes, direct filtration, filtrate recovery is directly used in preparation next time use, and filter cake is directly in 80 ℃ of dry products that obtain for 10 hours.
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 and is dissolved respectively, until temperature, is raised to after 30～80 ℃, adds unslaked lime or white lime, after turbulent flow circulates 60～240 minutes, and filtering separation; Filter cake in 80～120 ℃ dry 1～10 hour, in said process, 3～3.5 times of quality that boric acid is unslaked lime, or be 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, and primary particle is less than 100nm, and cluster granular size is between 5～10 μ m.
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| Application Number | Priority Date | Filing Date | Title |
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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 true CN103601208A (en) | 2014-02-26 |
| CN103601208B CN103601208B (en) | 2015-11-18 |
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| CN201310603617.8A Expired - Fee Related CN103601208B (en) | 2013-11-25 | 2013-11-25 | The preparation method of micro-nano structure boron calcium composite oxides |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103922391A (en) * | 2014-04-29 | 2014-07-16 | 武汉大学 | Preparation method of boron zinc composite oxide in micronano structure |
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Granted publication date: 20151118 Termination date: 20211125 |