CN101298333B - Preparation of 2ZnO.2B2O3.3.5H2O zinc borate - Google Patents
Preparation of 2ZnO.2B2O3.3.5H2O zinc borate Download PDFInfo
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- CN101298333B CN101298333B CN2008100482668A CN200810048266A CN101298333B CN 101298333 B CN101298333 B CN 101298333B CN 2008100482668 A CN2008100482668 A CN 2008100482668A CN 200810048266 A CN200810048266 A CN 200810048266A CN 101298333 B CN101298333 B CN 101298333B
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- 2zno
- water
- boric acid
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- zinc borate
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- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000004327 boric acid Substances 0.000 claims abstract description 16
- RZLVQBNCHSJZPX-UHFFFAOYSA-L zinc sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Zn+2].[O-]S([O-])(=O)=O RZLVQBNCHSJZPX-UHFFFAOYSA-L 0.000 claims abstract description 14
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 11
- 239000000047 product Substances 0.000 claims abstract description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000012065 filter cake Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000000706 filtrate Substances 0.000 claims abstract description 7
- 239000002351 wastewater Substances 0.000 abstract description 3
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 abstract description 2
- 239000003063 flame retardant Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- OMUGFZNEOIWQOD-UHFFFAOYSA-N boric acid;zinc Chemical compound [Zn].OB(O)O OMUGFZNEOIWQOD-UHFFFAOYSA-N 0.000 abstract 1
- 229940024464 emollients and protectives zinc product Drugs 0.000 abstract 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 4
- 229910052796 boron Inorganic materials 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
Abstract
本发明公开了一种2ZnO·2B2O3·3H2O硼酸锌的制备方法，该方法先将七水硫酸锌、硼酸与氨水或氢氧化钠按摩尔比为1∶2∶2溶于水中，在60～100℃温度下的某一温度恒温反应5～10小时，反应结束后，过滤，滤液回收，滤饼用热水洗然后烘干，即得到2ZnO·2B2O3·3H2O硼酸锌产品。本发明工艺简单，制备过程无废水排放，生产成本低，该产品用于阻燃材料，也可以用于日用化工、生物医药等领域。The invention discloses a preparation method of 2ZnO·2B 2 O 3 ·3H 2 O zinc borate. In the method, zinc sulfate heptahydrate, boric acid and ammonia water or sodium hydroxide are dissolved in water at a molar ratio of 1:2:2. , react at a constant temperature at a temperature of 60-100°C for 5-10 hours, after the reaction, filter, recover the filtrate, wash the filter cake with hot water and then dry it to obtain 2ZnO·2B 2 O 3 ·3H 2 O boric acid Zinc products. The invention has simple process, no waste water discharge in the preparation process, and low production cost. The product is used for flame-retardant materials, and can also be used in the fields of daily chemical industry, biomedicine and the like.
Description
技术领域technical field
本发明涉及一种2ZnO·2B2O3·3H2O硼酸锌的制备方法，属于无机材料领域。The invention relates to a preparation method of 2ZnO·2B 2 O 3 ·3H 2 O zinc borate, which belongs to the field of inorganic materials.
背景技术Background technique
根据文献报道，现有制备2ZnO·2B2O3·3H2O硼酸锌的方法为硼酸与氧化锌反应，该方法需要在配比中加入过量的硼酸，尽管母液可以重复利用，但还是存在硼损失和水排放以及硼含量的准确控制等问题[Amitava Choudhury，S.Neeraj，aSrinivasan Natarajan and C.N.R.Rao，An open-framework zincoborate formed byZn6B12O24clusters，J.Chem.Soc.，Dalton Trans.，2002，1535-1538]。According to literature reports, the existing method of preparing 2ZnO·2B 2 O 3 ·3H 2 O zinc borate is the reaction of boric acid and zinc oxide. This method needs to add excessive boric acid in the proportion. Although the mother liquor can be reused, there is still boron Issues such as loss and water discharge and accurate control of boron content [Amitava Choudhury, S. Neeraj, a Srinivasan Natarajan and CNRRao, An open-framework zincoborate formed by Zn6B12O24clusters, J.Chem.Soc., Dalton Trans., 2002, 1535-1538] .
发明内容Contents of the invention
本发明的目的在于提供一种2ZnO·2B2O3·3H2O硼酸锌的制备方法，该方法工艺过程简单、反应产率高、成本低、无废水排放，所得产品纯度高。The purpose of the present invention is to provide a preparation method of 2ZnO·2B 2 O 3 ·3H 2 O zinc borate, which has simple process, high reaction yield, low cost, no waste water discharge and high purity of the obtained product.
实现本发明的目的所采用的技术方案是：一种2ZnO·2B2O3·3H2O硼酸锌的制备方法先将七水硫酸锌、硼酸与氨水或氢氧化钠按摩尔比为1∶2∶2溶于水中，其中水和氨水的质量为七水硫酸锌和硼酸总质量的2～4倍；或者水的质量为硫酸锌、硼酸和氢氧化钠总质量的2～4倍，然后在60～100℃温度下的某一温度恒温充分反应，反应结束后，过滤，滤液回收，滤饼用热水洗然后烘干，即得到2ZnO·2B2O3·3H2O硼酸锌产品。The technical scheme adopted to realize the object of the present invention is: a kind of preparation method of 2ZnO 2B 2 O 3 3H 2 O zinc borate, first make zinc sulfate heptahydrate, boric acid and ammoniacal liquor or sodium hydroxide molar ratio be 1: 2 : 2 dissolved in water, wherein the quality of water and ammonia water is 2 to 4 times the total mass of zinc sulfate heptahydrate and boric acid; or the quality of water is 2 to 4 times the total mass of zinc sulfate, boric acid and sodium hydroxide, and then in A constant temperature of 60-100°C is used for full reaction. After the reaction, filter and recover the filtrate. The filter cake is washed with hot water and then dried to obtain 2ZnO·2B 2 O 3 ·3H 2 O zinc borate product.
上述所用氨水的质量百分比浓度为25～28％。The mass percent concentration of the ammonia water used above is 25-28%.
上述将七水硫酸锌、硼酸与氨水或氢氧化钠溶于水中，在60～100℃温度下的某一温度恒温反应5～10小时。The above-mentioned zinc sulfate heptahydrate, boric acid, ammonia water or sodium hydroxide are dissolved in water, and reacted at a constant temperature at a temperature of 60-100° C. for 5-10 hours.
与现有技术相比较，采用本发明的技术方案具有以下的优点：Compared with the prior art, adopting the technical scheme of the present invention has the following advantages:
本发明的制备方法工艺过程简单，反应产率高，制备过程无废水排放，充分利用反应物中的硼，减少了硼的损失，本发明生产成本低，特别适合工业生产。制得的2ZnO·2B2O3·3H2O硼酸锌产品用于阻燃材料，也可以用于日用化工、生物医药等领域。The preparation method of the invention has simple technological process, high reaction yield, no waste water discharge in the preparation process, fully utilizes boron in reactants, reduces boron loss, low production cost, and is especially suitable for industrial production. The prepared 2ZnO·2B 2 O 3 ·3H 2 O zinc borate product is used for flame retardant materials, and can also be used in fields such as daily chemical industry and biomedicine.
具体实施方式Detailed ways
实例1：分别称取12.3克七水硫酸锌和5.3克硼酸，加入65.00g水和5.8克质量百分比为28％氨水，混合搅拌，于70℃反应6小时，冷至室温后，反应结束后，过滤，滤液回收，滤饼用热水清洗，然后直接烘干，得到所需要的223硼酸锌产品。Example 1: Weigh 12.3 grams of zinc sulfate heptahydrate and 5.3 grams of boric acid respectively, add 65.00 grams of water and 5.8 grams of 28% ammonia by mass, mix and stir, react at 70°C for 6 hours, cool to room temperature, and after the reaction, Filtrate, recover the filtrate, wash the filter cake with hot water, and then directly dry it to obtain the required 223 zinc borate product.
实例2：分别取2.9克质量百分比为28％氨水和15克水，再称取6.15克七水硫酸锌和2.65克硼酸，混合搅拌，于98℃反应8小时，冷至室温后，过滤，滤液回收，滤饼用热水清洗，然后直接烘干得到所需要的223硼酸锌产品。Example 2: Take 2.9 grams of 28% ammonia water and 15 grams of water respectively, then weigh 6.15 grams of zinc sulfate heptahydrate and 2.65 grams of boric acid, mix and stir, react at 98°C for 8 hours, and filter after cooling to room temperature. Recovery, the filter cake is washed with hot water, and then directly dried to obtain the required 223 zinc borate product.
实例3：分别称取12.3克七水硫酸锌和5.3克硼酸，加入50克水、6.5克质量百分比为25％氨水，于85℃反应10小时，冷至室温后，过滤，滤液回收，滤饼用热水清洗，然后直接烘干，得到所需要的223硼酸锌产品。Example 3: Take 12.3 grams of zinc sulfate heptahydrate and 5.3 grams of boric acid respectively, add 50 grams of water, 6.5 grams of 25% ammonia by mass, react at 85°C for 10 hours, cool to room temperature, filter, reclaim the filtrate, and filter cake Wash with hot water, and then directly dry to obtain the required 223 zinc borate product.
实例4：分别称取12.3克七水硫酸锌和5.3克硼酸，加入60克水、3.4克氢氧化钠，于85℃反应10小时，冷至室温后，过滤，滤液回收，滤饼用热水清洗，然后直接烘干，得到所需要的223硼酸锌产品。Example 4: Weigh 12.3 grams of zinc sulfate heptahydrate and 5.3 grams of boric acid respectively, add 60 grams of water and 3.4 grams of sodium hydroxide, react at 85 ° C for 10 hours, cool to room temperature, filter, and recover the filtrate. The filter cake is washed with hot water Washing and then directly drying to obtain the required 223 zinc borate product.
Claims (5)
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008100482668A CN101298333B (en) | 2008-07-02 | 2008-07-02 | Preparation of 2ZnO.2B2O3.3.5H2O zinc borate |
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| CN2008100482668A CN101298333B (en) | 2008-07-02 | 2008-07-02 | Preparation of 2ZnO.2B2O3.3.5H2O zinc borate |
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| CN101298333B true CN101298333B (en) | 2010-06-30 |
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| CN104150501B (en) * | 2014-08-06 | 2016-05-11 | 中国科学院青海盐湖研究所 | A kind of zinc borate crystal whisker mother liquor is for the preparation of the method for Firebrake ZB crystal |
| CN109179445B (en) * | 2018-10-25 | 2022-02-18 | 青岛科技大学 | 2335 type zinc borate preparation and microstructure regulation method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1167730A (en) * | 1997-05-14 | 1997-12-17 | 武汉大学 | Process for preparing superfine zinc borate flame retardant |
| US6246083B1 (en) * | 1998-02-24 | 2001-06-12 | Micron Technology, Inc. | Vertical gain cell and array for a dynamic random access memory |
| CN1364142A (en) * | 2000-01-11 | 2002-08-14 | 水泽化学工业株式会社 | Zinc borate, and production and use thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1167730A (en) * | 1997-05-14 | 1997-12-17 | 武汉大学 | Process for preparing superfine zinc borate flame retardant |
| US6246083B1 (en) * | 1998-02-24 | 2001-06-12 | Micron Technology, Inc. | Vertical gain cell and array for a dynamic random access memory |
| CN1364142A (en) * | 2000-01-11 | 2002-08-14 | 水泽化学工业株式会社 | Zinc borate, and production and use thereof |
Non-Patent Citations (3)
| Title |
|---|
| JP特开平6-256013A 1994.09.13 |
| 刘少敏 等.生产低水硼酸锌现状的分析及新生产工艺的提出.《宁夏工学院学报（自然科学版）》.1996,第8卷(第4期),69-71. |
| 刘少敏等.生产低水硼酸锌现状的分析及新生产工艺的提出.《宁夏工学院学报(自然科学版)》.1996,第8卷(第4期),69-71. * |
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