CN1778868A - Production of nanometer zine borate fire retardant by zinc oxide and boric-acid solid-phase reaction - Google Patents
Production of nanometer zine borate fire retardant by zinc oxide and boric-acid solid-phase reaction Download PDFInfo
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- CN1778868A CN1778868A CN 200410046978 CN200410046978A CN1778868A CN 1778868 A CN1778868 A CN 1778868A CN 200410046978 CN200410046978 CN 200410046978 CN 200410046978 A CN200410046978 A CN 200410046978A CN 1778868 A CN1778868 A CN 1778868A
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- zinc oxide
- boric acid
- phase reaction
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- micron
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Abstract
Production of nanometer zinc borate fire retardant from zinc oxide and boric acid solid-phase reaction is carried out by ball grinding zinc oxide and boric acid into micro-zinc oxide and micro-boric acid, mixing the zinc oxide 60-80% with boric acid 20-40% proportional and grinding them into nanometer zinc borate from zinc oxide and boric acid. It has quantum size and composite effects.
Description
A method for preparing a nano zinc borate flame retardant by solid-phase reaction of zinc oxide and boric acid relates to a preparation method of a flame retardant, in particular to a preparation method of a zinc borate flame retardant.
The zinc borate is used as an important flame retardant, and according to literature search, the existing preparation process and method mainly comprise the following steps: us patent 5342553 discloses: reacting zinc oxide andboric acid which are used as raw materials at a boiling point; reacting borax, zinc sulfate and zinc oxide in an aqueous solution; at 2ZnO.2B2O3.5H2O and zinc oxide aqueous solution. Chinese patent 97109105 discloses a method for preparing zinc borate by reacting borax and zinc oxide in an aqueous solution. And so on. These wet methods have disadvantages of particle agglomeration and complicated preparation processes.
The invention aims to provide a method for preparing nano zinc borate by taking zinc oxide and boric acid as raw materials and using a solid-phase reaction. The zinc borate flame retardant prepared by the method has quantum size effect and composite effect.
The invention is realized by the following steps: firstly, respectively ball-milling zinc oxide and boric acid into micron-sized zinc oxide and micron-sized boric acid, and respectively adding 1-5% of surfactant or coupling agent by the total weight in the ball-milling process to prevent agglomeration, wherein the added surfactant can be sodium stearate, silane, polyvinyl acid, sodium acrylate or methyl methacrylate; the coupling agent can be silicon coupling agent, aluminate and alkoxy titanate; then, mixing the following raw materials by weight percent of 60-80% of zinc oxide: mixing the micron-sized zinc oxide and the micron-sized boric acid according to the proportion of 20-40% of boric acid, and grinding the mixture into the nano-sized zinc borate by utilizing the ball milling effect and the solid-phase reaction, wherein the reaction principle is as follows:
Due to the adoption of the scheme, the preparation method of the zinc borate is simple, and the prepared zinc borate flame retardant has a quantum size effect and a composite effect.
The present invention is described in detail below with reference to examples:
take the preparation of 100g of nano zinc borate as an example. Firstly, taking 80g of zinc oxide and 20g of boric acid, respectively ball-milling into micron-sized zinc oxide and micron-sized boric acid, and respectively adding 1g of sodium stearate in the ball-milling process: then, 80g of micron-sized zinc oxide and 20g of micron-sized boric acid are mixed, and are ground into nano-sized zinc borate by utilizing ball milling effect and solid-phase reaction, and 1g of sodium stearate is added in the grinding process.
Claims (3)
1. A method for preparing a nano zinc borate flame retardant by solid-phase reaction of zinc oxide and boric acid is characterized by comprising the following steps: firstly, respectively ball-milling zinc oxide and boric acid into micron-sized zinc oxide and micron-sized boric acid, and respectively adding 1-5% of surfactant or coupling agent by the total weight in the ball-milling process; then, mixing the following raw materials by weight percent of 60-80% of zinc oxide: 20 to 40 percent of boric acid, and grinding the micron-sized zinc oxide and the micron-sized boric acid into the nano-sized zinc borate by utilizing the ball milling effect and the solid phase reaction, wherein a surfactant or a coupling agent accounting for 1 to 5 percent of the total weight can be added in the ball milling process, or the ball milling is carried out under the vacuum condition.
2. The method for preparing the nano zinc borate flame retardant by the solid phase reaction of the zinc oxide and the boric acid, which is characterized by comprising the following steps: surfactants which may be added are sodium stearate, silanes, polyvinyl acid, sodium acrylate or methyl methacrylate.
3. The method for preparing the nano zinc borate flame retardant by the solid phase reaction of the zinc oxide and the boric acid, which is characterized by comprising the following steps: coupling agents which may be added are silicon coupling agents, aluminates or alkoxytitanates.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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CNB2004100469788A CN1306008C (en) | 2004-11-26 | 2004-11-26 | Production of nanometer zine borate fire retardant by zinc oxide and boric-acid solid-phase reaction |
Applications Claiming Priority (1)
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CNB2004100469788A CN1306008C (en) | 2004-11-26 | 2004-11-26 | Production of nanometer zine borate fire retardant by zinc oxide and boric-acid solid-phase reaction |
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CN1778868A true CN1778868A (en) | 2006-05-31 |
CN1306008C CN1306008C (en) | 2007-03-21 |
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CNB2004100469788A Expired - Fee Related CN1306008C (en) | 2004-11-26 | 2004-11-26 | Production of nanometer zine borate fire retardant by zinc oxide and boric-acid solid-phase reaction |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102634350A (en) * | 2012-03-28 | 2012-08-15 | 中国科学院过程工程研究所 | Preparation method of boron-containing flame retardant |
CN109734962A (en) * | 2019-01-11 | 2019-05-10 | 云南江磷集团股份有限公司 | Trbasic zinc phosphate, zinc borate microencapsulation Red Phosphorus Flame Retardant and preparation method thereof |
CN112105687A (en) * | 2018-05-14 | 2020-12-18 | 3M创新有限公司 | Controlled curing thermally conductive gap filling material |
Family Cites Families (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5122476B1 (en) * | 1971-02-24 | 1976-07-09 | ||
JPS59232901A (en) * | 1982-12-22 | 1984-12-27 | Agency Of Ind Science & Technol | Manufacture of boron nitride and substance containing boron nitride |
US5342553A (en) * | 1991-11-22 | 1994-08-30 | U. S. Borax Inc. | Process of making zinc borate and fire-retarding compositions thereof |
JPH06256013A (en) * | 1993-02-26 | 1994-09-13 | Hakusui Chem Ind Ltd | Production of zinc borate |
CN1167730A (en) * | 1997-05-14 | 1997-12-17 | 武汉大学 | Process for preparing superfine zinc borate flame retardant |
JP4669098B2 (en) * | 2000-01-11 | 2011-04-13 | 水澤化学工業株式会社 | Zinc borate, its production and use |
CN1417113A (en) * | 2001-11-06 | 2003-05-14 | 缪汉叶 | Mechanical process of producing superfine active zinc phosphate |
-
2004
- 2004-11-26 CN CNB2004100469788A patent/CN1306008C/en not_active Expired - Fee Related
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102634350A (en) * | 2012-03-28 | 2012-08-15 | 中国科学院过程工程研究所 | Preparation method of boron-containing flame retardant |
CN102634350B (en) * | 2012-03-28 | 2013-12-11 | 中国科学院过程工程研究所 | Preparation method of boron-containing flame retardant |
CN112105687A (en) * | 2018-05-14 | 2020-12-18 | 3M创新有限公司 | Controlled curing thermally conductive gap filling material |
CN109734962A (en) * | 2019-01-11 | 2019-05-10 | 云南江磷集团股份有限公司 | Trbasic zinc phosphate, zinc borate microencapsulation Red Phosphorus Flame Retardant and preparation method thereof |
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CN1306008C (en) | 2007-03-21 |
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Granted publication date: 20070321 |