CN111573624B - Method for preparing dodecahydrododecaboron disodium salt by using byproduct of decahydrododecaboron bistetraethylammonium salt - Google Patents
Method for preparing dodecahydrododecaboron disodium salt by using byproduct of decahydrododecaboron bistetraethylammonium salt Download PDFInfo
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- CN111573624B CN111573624B CN202010595281.5A CN202010595281A CN111573624B CN 111573624 B CN111573624 B CN 111573624B CN 202010595281 A CN202010595281 A CN 202010595281A CN 111573624 B CN111573624 B CN 111573624B
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B6/00—Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
- C01B6/06—Hydrides of aluminium, gallium, indium, thallium, germanium, tin, lead, arsenic, antimony, bismuth or polonium; Monoborane; Diborane; Addition complexes thereof
- C01B6/10—Monoborane; Diborane; Addition complexes thereof
- C01B6/13—Addition complexes of monoborane or diborane, e.g. with phosphine, arsine or hydrazine
- C01B6/15—Metal borohydrides; Addition complexes thereof
- C01B6/19—Preparation from other compounds of boron
- C01B6/21—Preparation of borohydrides of alkali metals, alkaline earth metals, magnesium or beryllium; Addition complexes thereof, e.g. LiBH4.2N2H4, NaB2H7
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- C01P2002/86—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by NMR- or ESR-data
Abstract
The invention relates to a method for preparing dodecahydrododecaboron disodium salt by using a byproduct of decahydrododecaboron bistetraethylammonium salt, belonging to the technical field of inorganic material synthesis processes. The method for preparing dodecahydrododecaboron disodium salt by utilizing the byproduct of decahydrododecaboron bistetraethylammonium salt comprises the following steps: dissolving a byproduct of decahydrododecaboron bistetraethylammonium salt with a solvent, reacting the dissolved byproduct with a sodium hydroxide solution, removing the solvent after the reaction is finished to obtain a dodecahydrododecaboron disodium salt crude product, dissolving the dodecahydrododecaboron disodium salt crude product, adding triethylamine hydrochloride solution to separate dodecahydrododecaboron triethylamine salt out, and reacting the dodecahydrododecaboron triethylamine salt with a sodium alkoxide solution to obtain the dodecahydrododecaboron triethylamine salt. The method for preparing dodecahydrododecaboron disodium salt by utilizing the byproduct of decahydrododecaboron bistetraethylammonium salt has the advantages of short reaction time, high yield, high efficiency, stable reaction process and safe operation.
Description
Technical Field
The invention belongs to the technical field of inorganic material synthesis processes, and particularly relates to a method for preparing dodecahydrododecaboron disodium salt by using a byproduct of decahydrododecaboron bistetraethylammonium salt.
Background
Dodecahydrododecaboron disodium salt having stable B12The skeleton has wide application in many fields, such as application as an energy storage material or application as a nontoxic medicine in boron neutron capture treatment.
The dodecahydrododecaboron disodium salt can be prepared by various methods, such as: adding sodium borohydride into diethylene glycol dimethyl ether in batches, heating to 100 ℃, reacting for a period of time, cooling to below 30 ℃, dropwise adding boron trifluoride ethyl ether, reacting for a period of time at normal temperature after dropwise adding is completed, heating to 100 ℃, reacting for a period of time under heat preservation, heating to 160 ℃, performing reflux reaction for 2 hours, cooling and supplementing sodium borohydride, continuing reflux reaction, cooling, filtering, evaporating filtrate to dryness to obtain a solid, dissolving the solid with water, and performing salt exchange to obtain a product. The preparation method has the following disadvantages: the 10L reactor generally needs 7 days from feeding to obtaining a finished product, the reaction time is long, the production efficiency is low, the obtained finished product is 20-30g, and the yield is low and is about 20-30%; the reaction temperature is high, hydrogen is released in the reaction process, and the operation risk coefficient is high; after the reaction is finished, the product is in the filtrate and is difficult to filter; the solid obtained after the filtrate is evaporated to dryness is added into water, so that the operation is dangerous, a large amount of heat and hydrogen can be discharged, and the treatment time is long.
In the prior art, other methods for preparing dodecahydrododecaboron disodium salt are available, which first use dimethyl glycol and NaBH4To obtain [ B ]12H12]2-Then Et was added3N, to obtain [ NEt3H]2[B12H12]Then [ NEt3H]2[B12H12]Reacting with sodium hydroxide to obtain Na2B12H12[Synthesis and characterization of synthetically useful salts of the weakly-coordinating dianion [B12Cl12]2-, Vanessa Geis, Kristin Guttsche, Carsten Knapp,Harald Scherer and Rabiya Uzun,Dalton Transactions,2009（15）]. The method still utilizes glycol dimethyl ether and NaBH4To obtain [ B ]12H12]2-Hydrogen is generated in the reaction process, and the operation is dangerous.
The byproducts of the decahydrododecaboron bistetraethylammonium salt contain dodecahydrododecaboron bistetraethylammonium salt, undedecahydroundedecaboron bistetraethylammonium salt, decahydrodecaboron bistetraethylammonium salt, nonahydrononaboron bistetraethylammonium salt and the like, wherein the dodecahydrododecaboron bistetraethylammonium salt accounts for about 80%, and the byproducts have no effective utilization way at present.
Disclosure of Invention
The invention aims to provide a method for preparing dodecahydrododecaboron disodium salt by utilizing a byproduct of decahydrododecaboron bistetraethylammonium salt, which has the advantages of short reaction time, high yield, high efficiency, stable reaction process and safe operation.
In order to achieve the above purpose, the invention adopts the technical scheme that:
the method for preparing dodecahydrododecaboron disodium salt by utilizing the byproduct of decahydrododecaboron bistetraethylammonium salt comprises the following steps: dissolving a byproduct of decahydrododecaboron bistetraethylammonium salt with a solvent, reacting the dissolved byproduct with sodium hydroxide, removing the solvent after the reaction is finished to obtain a dodecahydrododecaboron disodium salt crude product, dissolving the dodecahydrododecaboron disodium salt crude product, adding triethylamine hydrochloride to separate out dodecahydrododecaboron triethylamine salt, and reacting the dodecaboron dodecahydride triethylamine salt with sodium alcoholate to obtain the dodecahydrododecaboron triethylamine salt.
Further, the solvent for dissolving the byproduct of the decahydrodecaborane bistetraethylammonium salt is one of dimethyl sulfoxide, N-methylpyrrolidone and 2-pyrrolidone.
Further, the ratio of the byproduct of the decahydrodecaborobistetraethylammonium salt to the solvent is 1 (3-12). Preferably, the ratio of the byproduct of the decahydrododecaboron bistetraethylammonium salt to the solvent is 1 (6-8).
Further, the reaction temperature of the dissolved by-product of the decahydrodecaborane bistetraethylammonium salt and sodium hydroxide is 110-140 ℃, and the reaction time is 6-10 h.
Further, the molar ratio of the byproduct of the decahydrodecaborobistetraethylammonium salt to the sodium hydroxide is 1 (2-5). Preferably, the molar ratio of the byproduct of the decahydrodecaborobistetraethylammonium salt to the sodium hydroxide is 1 (2-3).
Further, when the dodecahydrododecaboron triethylamine salt reacts with sodium alcoholate, the temperature is firstly raised to reflux reaction for 0.1-2h, and then the temperature is lowered to end the reflux.
Further, the molar ratio of the dodecahydrododecaboron triethylamine salt to the sodium alcoholate is 1 (0.95-1.03).
Further, the sodium alkoxide is sodium methoxide or sodium ethoxide.
And calculating the adding amount of the solvent, the sodium hydroxide and the sodium alkoxide by taking the dodecahydrododecahydrododecaboron bistetraethylammonium salt in the byproducts of the decahydrododecaboron bistetraethylammonium salt, namely calculating the molar mass of the byproducts of the decahydrododecaboron bistetraethylammonium salt, and calculating the molar mass of the byproducts of the decahydrododecaboron bistetraethylammonium salt by the molar mass of the pure dodecahydrododecaboron bistetraethylammonium salt.
The invention has the beneficial effects that:
the method for preparing the dodecahydrododecaboron disodium salt by using the byproduct of the decahydrododecaboron bistetraethylammonium salt has the advantages that the raw material is the byproduct of the decahydrododecaboron bistetraethylammonium salt, no effective utilization way is available at present, the dodecahydrododecaboron bistetraethylammonium salt accounts for about 80%, the dodecahydrododecaboron disodium salt prepared by using the bistetraethylammonium dodecahydrododecaborate belongs to the reutilization of the byproduct, the environment is protected, and the energy is saved.
According to the method for preparing dodecahydrododecaboron disodium salt by utilizing the byproduct of decahydrododecaboron bistetraethylammonium salt, the dodecahydrododecaboron disodium salt crude product contains various impurities such as undedecahydroundecabron disodium salt, decahydrododecaboron disodium salt, nonahydrononaboron disodium salt and the like, and after triethylamine hydrochloride is added, dodecahydrododecaboron triethylamine salt is separated out because of insolubility of water, so that pure dodecahydrododecaboron triethylamine salt is obtained. Because dodecahydrododecaboron triethylamine salt is insoluble in water, sodium alcoholate is selected to react with dodecahydrododecaboron triethylamine salt to obtain dodecahydrododecaboron disodium salt.
The method for preparing dodecahydrododecaboron disodium salt by utilizing the byproduct of decahydrododecaboron bistetraethylammonium salt has the advantages of short reaction time, high yield, stable reaction process, no hydrogen gas emission and safe operation.
Drawings
FIG. 1 shows the preparation of disodium dodecahydrododecaboron salt obtained in example 111B NMR chart.
Detailed Description
The present invention will be further described with reference to the following embodiments and accompanying drawings.
Example 1
The method for preparing dodecahydrododecaboron disodium salt by using the byproduct of decahydrododecaboron bistetraethylammonium salt comprises the following steps:
1) 300g of a byproduct of decahydrodecaborane bistetraethylammonium salt, 3.5L of dimethyl sulfoxide, sodium hydroxide and 100ml of water are added into a 10L four-mouth bottle, and the temperature is raised to 120 ℃ for reaction for 8 hours with heat preservation. And (3) distilling the solvent dimethyl sulfoxide by an oil pump under reduced pressure to obtain a crude product of dodecahydrododecaboron disodium salt. The molar ratio of the by-product of decahydrodecaboron bistetraethylammonium salt to sodium hydroxide was 1: 5. In the byproduct of the decahydrododecaboron bistetraethylammonium salt, the mass percentage of dodecahydrododecaboron bistetraethylammonium salt is 82%.
2) Adding the crude dodecahydrododecaboron disodium salt obtained in the step 1) into 2L of water, stirring to dissolve the crude dodecahydrododecaboron disodium salt, and filtering to remove insoluble substances. Adding triethylamine hydrochloride into the filtrate in batches until no solid is separated out, and then filtering to obtain solid dodecahydrododecaboron triethylamine salt for later use.
3) Adding sodium methoxide into a 5L four-mouth bottle, and then adding dodecahydrododecaboron triethylamine salt obtained in the step 2), wherein the molar ratio of the dodecahydrododecaboron triethylamine salt to the sodium methoxide is 1: 1.03. Heating to reflux reaction for 30min, cooling to reflux, filtering, concentrating the filtrate, dispersing and filtering the concentrated filtrate with chloroform, and removing residual organic solvent to obtain white solid, namely 109.6g of dodecahydrododecaboron disodium salt, the purity of which is 97 percent, and the yield of which is 93.0 percent.
And calculating the adding amount of dimethyl sulfoxide, sodium hydroxide and sodium methoxide by taking the dodecahydrododecahydrododecaboron bistetraethylammonium salt in the byproducts of the decahydrododecaboron bistetraethylammonium salt, namely calculating the molar amount of the byproducts of the decahydrododecaboron bistetraethylammonium salt, and calculating the molar mass of the byproducts of the decahydrododecaboron bistetraethylammonium salt based on the molar mass of the pure dodecahydrododecaboron bistetraethylammonium salt.
Example 2
The method for preparing dodecahydrododecaboron disodium salt by using the byproduct of decahydrododecaboron bistetraethylammonium salt comprises the following steps:
1) 300g of a byproduct of decahydrodecaborane bis-tetraethylammonium salt, 2L of dimethyl sulfoxide, sodium hydroxide and 100ml of water are added into a 10L four-mouth bottle, and the temperature is raised to 110 ℃ for reaction for 10 hours with heat preservation. And (3) distilling the solvent dimethyl sulfoxide by an oil pump under reduced pressure to obtain a crude product of dodecahydrododecaboron disodium salt. The molar ratio of the by-product of decahydrodecaboron bistetraethylammonium salt to sodium hydroxide was 1: 3. In the byproduct of the decahydrododecaboron bistetraethylammonium salt, the mass percentage of dodecahydrododecaboron bistetraethylammonium salt is 80%.
2) Adding the crude dodecahydrododecaboron disodium salt obtained in the step 1) into 2L of water, stirring to dissolve the crude dodecahydrododecaboron disodium salt, and filtering to remove insoluble substances. Adding triethylamine hydrochloride into the filtrate in batches until no solid is separated out, and then filtering to obtain solid dodecahydrododecaboron triethylamine salt for later use.
3) Adding sodium methoxide into a 5L four-mouth bottle, and then adding dodecahydrododecaboron triethylamine salt obtained in the step 2), wherein the molar ratio of the dodecahydrododecaboron triethylamine salt to the sodium methoxide is 1: 0.98. Heating to reflux reaction for 60min, cooling to reflux, filtering, concentrating the filtrate, dispersing and filtering the concentrated filtrate with chloroform, and removing residual organic solvent to obtain white solid, namely 123.7g of dodecahydrododecaboron disodium salt, with the purity of 98% and the yield of 92.5%.
And calculating the adding amount of dimethyl sulfoxide, sodium hydroxide and sodium methoxide by taking the dodecahydrododecahydrododecaboron bistetraethylammonium salt in the byproducts of the decahydrododecaboron bistetraethylammonium salt, namely calculating the molar amount of the byproducts of the decahydrododecaboron bistetraethylammonium salt, and calculating the molar mass of the byproducts of the decahydrododecaboron bistetraethylammonium salt based on the molar mass of the pure dodecahydrododecaboron bistetraethylammonium salt.
Example 3
The method for preparing dodecahydrododecaboron disodium salt by using the byproduct of decahydrododecaboron bistetraethylammonium salt comprises the following steps:
1) 300g of a byproduct of decahydrodecaborane bistetraethylammonium salt, 0.8L of dimethyl sulfoxide, sodium hydroxide and 100ml of water are added into a 10L four-mouth bottle, and the temperature is raised to 140 ℃ for heat preservation reaction for 6 h. And (3) distilling the solvent dimethyl sulfoxide by an oil pump under reduced pressure to obtain a crude product of dodecahydrododecaboron disodium salt. The molar ratio of the by-product of decahydrodecaboron bistetraethylammonium salt to sodium hydroxide was 1: 2. In the byproduct of the decahydrododecaboron bistetraethylammonium salt, the mass percentage of dodecahydrododecaboron bistetraethylammonium salt is 82%.
2) Adding the crude dodecahydrododecaboron disodium salt obtained in the step 1) into 2L of water, stirring to dissolve the crude dodecahydrododecaboron disodium salt, and filtering to remove insoluble substances. Adding triethylamine hydrochloride into the filtrate in batches until no solid is separated out, and then filtering to obtain solid dodecahydrododecaboron triethylamine salt for later use.
3) Adding sodium ethoxide into a 5L four-mouth bottle, and then adding dodecahydrododecaboron triethylamine salt obtained in the step 2), wherein the molar ratio of dodecahydrododecaboron triethylamine salt to sodium ethoxide is 1: 1. Heating to reflux reaction for 120min, cooling to reflux, filtering, concentrating the filtrate, dispersing and filtering the concentrated filtrate with chloroform, and removing residual organic solvent to obtain white solid, namely dodecahydrododecaboron disodium salt 112.6g, the purity of 97%, and the yield of 95.0%.
And calculating the addition amount of dimethyl sulfoxide, sodium hydroxide and sodium ethoxide by taking the dodecahydrododecaboron bistetraethylammonium salt in the byproducts of the decahydrododecaboron bistetraethylammonium salt, namely calculating the molar mass of the byproducts of the decahydrododecaboron bistetraethylammonium salt, and calculating the molar mass of the byproducts of the decahydrododecaboron bistetraethylammonium salt based on the molar mass of the pure dodecahydrododecaboron bistetraethylammonium salt.
Example 4
The method for preparing dodecahydrododecaboron disodium salt by using the byproduct of decahydrododecaboron bistetraethylammonium salt comprises the following steps:
1) 300g of a byproduct of decahydrodecaborane bistetraethylammonium salt, 1.5L of 2-pyrrolidone, sodium hydroxide and 100ml of water are added into a 10L four-mouth bottle, and the temperature is raised to 130 ℃ for heat preservation reaction for 6 h. And (3) distilling the solvent 2-pyrrolidone by an oil pump under reduced pressure to obtain a crude product of dodecahydrododecaboron disodium salt. The molar ratio of the by-product of decahydrodecaboron bistetraethylammonium salt to sodium hydroxide was 1: 3. In the byproduct of the decahydrododecaboron bistetraethylammonium salt, the mass percentage of dodecahydrododecaboron bistetraethylammonium salt is 85%.
2) Adding the crude dodecahydrododecaboron disodium salt obtained in the step 1) into 2L of water, stirring to dissolve the crude dodecahydrododecaboron disodium salt, and filtering to remove insoluble substances. Adding triethylamine hydrochloride into the filtrate in batches until no solid is separated out, and then filtering to obtain solid dodecahydrododecaboron triethylamine salt for later use.
3) Adding sodium ethoxide into a 5L four-mouth bottle, and then adding dodecahydrododecaboron triethylamine salt obtained in the step 2), wherein the molar ratio of the dodecahydrododecaboron triethylamine salt to the sodium ethoxide is 1: 1.01. Heating to reflux reaction for 90min, cooling to reflux, filtering, concentrating the filtrate, dispersing and filtering the concentrated filtrate with chloroform, and removing residual organic solvent to obtain white solid, i.e. 113.1g of dodecahydrododecaboron disodium salt, with the purity of 98% and the yield of 93.0%.
And calculating the adding amount of the 2-pyrrolidone, the sodium hydroxide and the sodium ethoxide by taking the dodecahydrododecaboron bistetraethylammonium salt in the byproducts of the decahydrododecaboron bistetraethylammonium salt, namely calculating the molar weight of the byproducts of the decahydrododecaboron bistetraethylammonium salt, and calculating the molar weight of the byproducts of the decahydrododecaboron bistetraethylammonium salt by the molar weight of the pure dodecahydrododecaboron bistetraethylammonium salt.
Example 5
The method for preparing dodecahydrododecaboron disodium salt by using the byproduct of decahydrododecaboron bistetraethylammonium salt comprises the following steps:
1) 300g of a by-product of decahydrodecaborane bistetraethylammonium salt, 3L N-methyl pyrrolidone, sodium hydroxide and 100ml of water are added into a 10L four-mouth bottle, and the temperature is raised to 120 ℃ for reaction for 8 hours with heat preservation. And (3) distilling the solvent N-methyl pyrrolidone by an oil pump under reduced pressure to obtain a crude product of dodecahydrododecaboron disodium salt. The molar ratio of the by-product of decahydrodecaboron bistetraethylammonium salt to sodium hydroxide was 1: 5. The mass percentage of the dodecahydrododecaboron bistetraethylammonium in the byproduct of decahydrododecaboron bistetraethylammonium salt is 81%.
2) Adding the crude dodecahydrododecaboron disodium salt obtained in the step 1) into 2L of water, stirring to dissolve the crude dodecahydrododecaboron disodium salt, and filtering to remove insoluble substances. Adding triethylamine hydrochloride into the filtrate in batches until no solid is separated out, and then filtering to obtain solid dodecahydrododecaboron triethylamine salt for later use.
3) Adding sodium methoxide into a 5L four-mouth bottle, and then adding dodecahydrododecaboron triethylamine salt obtained in the step 2), wherein the molar ratio of the dodecahydrododecaboron triethylamine salt to the sodium methoxide is 1: 0.95. Heating to reflux reaction for 60min, cooling to reflux, filtering, concentrating the filtrate, dispersing and filtering the concentrated filtrate with chloroform, and removing residual organic solvent to obtain white solid, namely 106.1g of dodecahydrododecaboron disodium salt, with the purity of 98.5% and the yield of 92.0%.
And calculating the adding amount of N-methylpyrrolidone, sodium hydroxide and sodium methoxide by taking the dodecahydrododecaboron bistetraethylammonium salt in the byproducts of the decahydrododecaboron bistetraethylammonium salt, namely calculating the molar weight of the byproducts of the decahydrododecaboron bistetraethylammonium salt, and calculating the molar weight of the byproducts of the decahydrododecaboron bistetraethylammonium salt based on the molar weight of the pure dodecahydrododecaboron bistetraethylammonium salt.
Test example 1
The boron dodecahydrododecaborate disodium salt prepared in example 1 of the present invention was subjected to nuclear magnetic resonance boron spectroscopy, and the results are shown in fig. 1.
Claims (4)
1. The method for preparing dodecahydrododecaboron disodium salt by utilizing the byproduct of decahydrododecaboron bistetraethylammonium salt is characterized by comprising the following steps: dissolving a byproduct of decahydrododecaboron bistetraethylammonium salt with a solvent, and then reacting the dissolved byproduct with sodium hydroxide, wherein the molar ratio of the byproduct of decahydrododecaboron bistetraethylammonium salt to sodium hydroxide is 1 (2-5), the solvent is one of dimethyl sulfoxide, N-methylpyrrolidone and 2-pyrrolidone, removing the solvent after the reaction is finished to obtain a dodecahydrododecaboron disodium salt crude product, adding triethylamine hydrochloride after the dodecahydrododecaboron disodium salt crude product is dissolved to separate dodecahydrododecaboron triethylamine salt out, and reacting the dodecaboron hydrododecaamine salt with sodium alkoxide to obtain the dodecaboron hydrododecaboron triethylamine salt/sodium alkoxide molar ratio of 1 (0.95-1.03).
2. The method for preparing dodecahydrododecaboron disodium salt by using the byproduct of decahydrododecaboron bistetraethylammonium salt according to claim 1, wherein the mass ratio of the byproduct of decahydrododecaboron bistetraethylammonium salt to the solvent is 1 (3-12).
3. The method for preparing dodecahydrododecaboron disodium salt by using the byproduct of decahydrododecaboron bistetraethylammonium salt as claimed in claim 1, wherein the reaction temperature of the dissolved byproduct of decahydrododecaboron bistetraethylammonium salt with sodium hydroxide is 110-140 ℃, and the reaction time is 6-10 h.
4. The method for preparing dodecahydrododecaboron disodium salt by using the byproduct of decahydrododecaboron bistetraethylammonium salt according to claim 1, wherein when the dodecahydrododecaboron triethylamine salt is reacted with sodium alkoxide, the temperature is first raised to reflux reaction for 0.1-2h, and then the temperature is lowered to end the reflux.
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