CN101210026A - Method for preparing sodium tetraphenylborate - Google Patents
Method for preparing sodium tetraphenylborate Download PDFInfo
- Publication number
- CN101210026A CN101210026A CNA2006101487208A CN200610148720A CN101210026A CN 101210026 A CN101210026 A CN 101210026A CN A2006101487208 A CNA2006101487208 A CN A2006101487208A CN 200610148720 A CN200610148720 A CN 200610148720A CN 101210026 A CN101210026 A CN 101210026A
- Authority
- CN
- China
- Prior art keywords
- preparation
- sodium tetraphenylborate
- magnesium
- grignard reagent
- chlorobenzene
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
The invention relates to a preparation method of sodium tetraphenylboron, which uses magnesium and chlorobenzene as raw materials for preparing Grignard reagent; the Grignard reagent reacts with boron trifluoride ether solution to synthesize tetraphenyl boron magnesium chloride that is hydrolyzed by sodium carbonate and then the sodium tetraphenylboron is obtained. The preparation method of the sodium tetraphenylboron of the invention has high conversion rate, high purity of the obtained product and safe and controllable production process, for no aether is used as solvent, thus being suitable for mass production.
Description
Technical field
The present invention relates to a kind of preparation method of chemical reagent, relate in particular to a kind of preparation method of sodium tetraphenylborate.
Background technology
Sodium tetraphenylborate is a kind of analytical reagent, is mainly used in the potassium concn of measuring in the blood, can be used to remove the metal caesium in addition.The preparation method of prior art sodium tetraphenylborate is for being that starting raw material prepares Grignard reagent with chlorobenzene or bromobenzene, reacts in diethyl ether solution or tetrahydrofuran solution with boron trifluoride then to make.But the ether boiling point is low, and big production has certain danger, and the tetrahydrofuran (THF) price is more expensive, and the rate of recovery is low.
Summary of the invention
Purpose of the present invention is to solve the problems referred to above that prior art exists, and a kind of preparation method of new sodium tetraphenylborate is provided.
The object of the present invention is achieved like this: a kind of preparation method of sodium tetraphenylborate may further comprise the steps:
A, preparation Grignard reagent
With magnesium and chlorobenzene is reactant, is action solvent with dry toluene and tetrahydrofuran (THF), is catalyzer with iodine, prepares Grignard reagent;
B, synthetic tetraphenylphosphonichloride chloride boron magnesium
In steps A gained Grignard reagent, add the diethyl ether solution reaction of toluene and boron trifluoride, synthesize tetraphenylphosphonichloride chloride boron magnesium;
C, preparation sodium tetraphenylborate
With the yellow soda ash hydrolysis of step B gained tetraphenylphosphonichloride chloride boron magnesium, prepare sodium tetraphenylborate.
In the reactant described in the steps A, the consumption of magnesium is excessive with respect to chlorobenzene.
In the action solvent described in the steps A, the proportioning of dry toluene and tetrahydrofuran (THF) is 1～6: 1.
The add-on of the diethyl ether solution of the boron trifluoride described in the step B (weight) be the reactant chlorobenzene consumption (weight) 20%～100%; The add-on of toluene (volume) be the diethyl ether solution of boron trifluoride add-on (volume) 50%～100%.
The consumption of the yellow soda ash described in the step C is excessive with respect to tetraphenylphosphonichloride chloride boron magnesium.
Preparation method's transformation efficiency height of sodium tetraphenylborate of the present invention, prepared product purity height, and also owing to do not use ether, production process safety is controlled, is suitable for scale operation.
Embodiment
Embodiment 1:
The dry toluene that in the 500mL exsiccant four-hole boiling flask of reflux condensing tube, dropping funnel and thermometer is housed, adds magnesium sheet 10 grams, a few granule iodine and 80mL, heating, slowly drip the mixture of the tetrahydrofuran (THF) of 40mL chlorobenzene and 40mL, make the maintenance reflux state, refluxed again two hours after dripping end, prepare Grignard reagent.
Above-mentioned reaction solution is cooled to about 30 ℃, slowly drips 10mL toluene and 20mL boron trifluoride ether solution, drip to finish back insulation reaction half an hour, then reaction solution is reduced to about 30 ℃.Synthesize tetraphenylphosphonichloride chloride boron magnesium.
Above-mentioned reaction solution is slowly poured in the 300mL frozen water, in reaction solution, added soda ash 50 grams then, stirred 1 hour, standing demix, water layer merges organic phase with the methylbenzene extraction of 10mL, dehydrates with 5 gram soda ash.Concentrate, crystallisation by cooling filters, and uses the toluene rinsing, uses petroleum ether at last, is drying to obtain sodium tetraphenylborate product 21.0 grams of the present invention, content＞99.0%.
Embodiment 2:
The dry toluene that in the 500mL exsiccant four-hole boiling flask of reflux condensing tube, dropping funnel and thermometer is housed, adds magnesium sheet 10 grams, a few granule iodine and 120mL, heating, slowly drip the mixture of the tetrahydrofuran (THF) of 40mL chlorobenzene and 40mL, make the maintenance reflux state, refluxed again two hours after dripping end, prepare Grignard reagent.
Above-mentioned reaction solution is cooled to about 30 ℃, slowly drips 20mL toluene and 30mL boron trifluoride ether solution, drip to finish back insulation reaction half an hour, then reaction solution is reduced to about 30 ℃.Synthesize tetraphenylphosphonichloride chloride boron magnesium.
Above-mentioned reaction solution is slowly poured in the 300mL frozen water, in reaction solution, added soda ash 50 grams then, stirred 1 hour, standing demix, water layer merges organic phase with the methylbenzene extraction of 10mL, dehydrates with 5 gram soda ash.Concentrate, crystallisation by cooling filters, and uses the toluene rinsing, uses petroleum ether at last, is drying to obtain sodium tetraphenylborate product 23.5 grams of the present invention, content＞99.0%.
Embodiment 3:
The dry toluene that in the 500mL exsiccant four-hole boiling flask of reflux condensing tube, dropping funnel and thermometer is housed, adds magnesium sheet 10 grams, a few granule iodine and 180mL, heating, slowly drip the mixture of the tetrahydrofuran (THF) of 40mL chlorobenzene and 40mL, make the maintenance reflux state, refluxed again two hours after dripping end, prepare Grignard reagent.
Above-mentioned reaction solution is cooled to about 30 ℃, slowly drips 40mL toluene and 40mL boron trifluoride ether solution, drip to finish back insulation reaction half an hour, then reaction solution is reduced to about 30 ℃.Synthesize tetraphenylphosphonichloride chloride boron magnesium.
Above-mentioned reaction solution is slowly poured in the 300mL frozen water, in reaction solution, added soda ash 50 grams then, stirred 1 hour, standing demix, water layer merges organic phase with the methylbenzene extraction of 10mL, dehydrates with 5 gram soda ash.Concentrate, crystallisation by cooling filters, and uses the toluene rinsing, uses petroleum ether at last, is drying to obtain sodium tetraphenylborate product 24.5 grams of the present invention, content＞99.0%.
Claims (5)
1. the preparation method of a sodium tetraphenylborate is characterized in that: may further comprise the steps:
A, preparation Grignard reagent
With magnesium and chlorobenzene is reactant, is action solvent with dry toluene and tetrahydrofuran (THF), is catalyzer with iodine, prepares Grignard reagent;
B, synthetic tetraphenylphosphonichloride chloride boron magnesium
In steps A gained Grignard reagent, add the diethyl ether solution reaction of toluene and boron trifluoride, synthesize tetraphenylphosphonichloride chloride boron magnesium;
C, preparation sodium tetraphenylborate
With the yellow soda ash hydrolysis of step B gained tetraphenylphosphonichloride chloride boron magnesium, prepare sodium tetraphenylborate.
2. the preparation method of sodium tetraphenylborate as claimed in claim 1, it is characterized in that: in the reactant described in the steps A, the consumption of magnesium is excessive with respect to chlorobenzene.
3. the preparation method of sodium tetraphenylborate as claimed in claim 1, it is characterized in that: in the action solvent described in the steps A, the proportioning of dry toluene and tetrahydrofuran (THF) is 1～6: 1.
4. the preparation method of sodium tetraphenylborate as claimed in claim 1 is characterized in that: the add-on of the diethyl ether solution of the boron trifluoride described in the step B (weight) is 20%～100% of the consumption (weight) of reactant chlorobenzene; The add-on of toluene (volume) be the diethyl ether solution of boron trifluoride add-on (volume) 50%～100%.
5. the preparation method of sodium tetraphenylborate as claimed in claim 1, it is characterized in that: the consumption of the yellow soda ash described in the step C is excessive with respect to tetraphenylphosphonichloride chloride boron magnesium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006101487208A CN101210026A (en) | 2006-12-30 | 2006-12-30 | Method for preparing sodium tetraphenylborate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006101487208A CN101210026A (en) | 2006-12-30 | 2006-12-30 | Method for preparing sodium tetraphenylborate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101210026A true CN101210026A (en) | 2008-07-02 |
Family
ID=39610295
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2006101487208A Pending CN101210026A (en) | 2006-12-30 | 2006-12-30 | Method for preparing sodium tetraphenylborate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101210026A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103212388A (en) * | 2013-04-23 | 2013-07-24 | 中国科学院青海盐湖研究所 | Gel ball type rubidium/caesium ion adsorbent, and preparation method and application thereof |
| US20150311565A1 (en) * | 2014-04-28 | 2015-10-29 | Toyota Motor Engineering & Manufacturing North America, Inc. | Chloride-free electrolyte for a magnesium battery and a method to convert a magnesium electrolyte to a chloride-free electrolyte |
| CN111312428A (en) * | 2019-12-27 | 2020-06-19 | 刘荣华 | Conductive aluminum paste for solar cell and preparation method thereof |
-
2006
- 2006-12-30 CN CNA2006101487208A patent/CN101210026A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103212388A (en) * | 2013-04-23 | 2013-07-24 | 中国科学院青海盐湖研究所 | Gel ball type rubidium/caesium ion adsorbent, and preparation method and application thereof |
| CN103212388B (en) * | 2013-04-23 | 2015-03-25 | 中国科学院青海盐湖研究所 | Gel ball type rubidium/caesium ion adsorbent, and preparation method and application thereof |
| US20150311565A1 (en) * | 2014-04-28 | 2015-10-29 | Toyota Motor Engineering & Manufacturing North America, Inc. | Chloride-free electrolyte for a magnesium battery and a method to convert a magnesium electrolyte to a chloride-free electrolyte |
| US10147970B2 (en) * | 2014-04-28 | 2018-12-04 | Toyota Motor Engineering & Manufacturing North America, Inc. | Chloride-free electrolyte for a magnesium battery and a method to convert a magnesium electrolyte to a chloride-free electrolyte |
| CN111312428A (en) * | 2019-12-27 | 2020-06-19 | 刘荣华 | Conductive aluminum paste for solar cell and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104530106A (en) | Method for preparing arylboronic acid compound | |
| CN102241662A (en) | Synthetic method of thiophene-3-ethanol | |
| CN103694119A (en) | Preparation method of ethyl 4,4,4-trifluoroacetoacetate | |
| CN101210026A (en) | Method for preparing sodium tetraphenylborate | |
| CN102295519A (en) | Preparation method for iodomethane | |
| CN102757455B (en) | Preparation method of cyclopropylboronic acid | |
| CN103058984B (en) | Synthesis method of watermelon ketone | |
| CN102992959A (en) | Method for preparing aluminium isopropoxide by using high water content isopropanol | |
| CN103044473B (en) | Method for preparing cyclopropylboric acid | |
| CN105085158A (en) | Synthesis method of methyl benzotrifluoride | |
| CN107759445A (en) | One kind prepares 1（3,3, Dimethylcyclohexyl）The method of ethanol | |
| CN105111039A (en) | Preparation method of chloroisopentene | |
| CN102964233A (en) | Synthetic method of 3,5-2-fluoro-(trifluoromethyl)benzophenone | |
| CN101370759B (en) | Method for producing halogen-substituted benzenedimethanol | |
| CN101665511B (en) | Method of synthesizing tetraalkyltin | |
| CN101012154A (en) | Method of preparing citronellol | |
| CN102532038B (en) | Method for preparing 2-methyl-1-pyrimidine-5-yl-1-(4-fluoroform methoxyl phenyl) allene-1-alcohol | |
| CN102659520B (en) | Synthetic method of 2,3,5,6-tetrafluorobenzyl alcohol | |
| CN106365951A (en) | 2-bromopropane recycling and reuse process in preparation process of 2,2-Diisopropylpropionitrile | |
| CN101775029A (en) | Convenient synthesis method for alkyl substitution phenyloboricacid | |
| CN101863732B (en) | Synthesis method of end-group alkyne | |
| CN104592283A (en) | Synthetic method of silane coupling agent Si-69 | |
| CN107814687A (en) | A kind of synthetic method to chlorophenethylol | |
| CN106554259B (en) | A kind of preparation method of 3- aryl propyl alcohol | |
| CN102093399A (en) | Novel boronizing agent dimethylamino boronic acid pinacol ester as well as synthesis and application of novel boronizing agent dimethylamino boronic acid pinacol ester |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20080702 |