CN105314644A - Preparation method of boron trifluoride dihydrate - Google Patents

Preparation method of boron trifluoride dihydrate Download PDF

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Publication number
CN105314644A
CN105314644A CN201510907686.7A CN201510907686A CN105314644A CN 105314644 A CN105314644 A CN 105314644A CN 201510907686 A CN201510907686 A CN 201510907686A CN 105314644 A CN105314644 A CN 105314644A
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China
Prior art keywords
boron trifluoride
deionized water
preparation
reaction
complex
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CN201510907686.7A
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Chinese (zh)
Inventor
刘雅婷
徐三善
高飞
张宇
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Jiujiang Tianci High & New Material Co Ltd
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Jiujiang Tianci High & New Material Co Ltd
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Priority to CN201510907686.7A priority Critical patent/CN105314644A/en
Publication of CN105314644A publication Critical patent/CN105314644A/en
Pending legal-status Critical Current

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Abstract

The invention concretely relates to a preparation method of a boron trifluoride dihydrate. The preparation method comprises the following steps of firstly, adding deionized water into a reactor, and carrying out cooling treatment outside the reactor; and secondly, introducing boron trifluoride to the deionized water in the reactor, and enabling boron trifluoride and the deionized water to be subjected to complex reaction to prepare the boron trifluoride dihydrate. Compared with the prior art, the preparation method of the boron trifluoride dihydrate, provided by the invention, has the advantages that a boron trifluoride complex, namely the boron trifluoride dehydrate, prepared by complex reaction of water vapor and boron trifluoride gases by taking the deionized water as a medium, is low in cost and environment-friendly because no organic solvents are used; and the complex reaction is carried out at normal temperature or slightly high temperature, and therefore, the reaction is mild, and the reaction condition is more easily controlled and is safer.

Description

A kind of preparation method of boron trifluoride two hydrate
Technical field
The present invention relates to chemical production field, particularly relate to a kind of preparation method of boron trifluoride complex.
Background technology
Boron trifluoride complex is a kind of important industrial raw material, can be used as various catalyzer and uses.In the prior art, the preparation method of boron trifluoride complex is that the steam of such as ether, tetrahydrofuran (THF) carries out complex reaction with boron trifluoride and organic vapor.Wherein, the reaction equation of etherate is: BF 3+ O (CH 2) 4→ BF 3o (CH 2) 4; The reaction equation of tetrahydrofuran complex is: BF 3+ O (CH 2cH 3) 2→ BF 3o (CH 2cH 3) 2.
Such as, application publication number is " CN102911195A ", patent name be " preparation method of boron trifluoride tetrahydrofuran " in first patent of invention, adopt tetrahydrofuran (THF) steam to prepare boron trifluoride complex.In above-mentioned patent, exothermic heat of reaction, the more difficult control of temperature, and the ether organic solvents such as tetrahydrofuran (THF), easily produce superoxide and boiling point is low, belongs to inflammable explosive article, there is certain potential safety hazard in commercial process.
Summary of the invention
The object of the present invention is to provide a kind of deionized water that adopts to produce the method for boron trifluoride complex as medium, the method is carried out under cryogenic, safe and environmentally friendly.
For achieving the above object, the invention provides a kind of preparation method of boron trifluoride two hydrate, comprise the following steps:
Step one, adds deionized water in the reactor, and cooling process is carried out in reactor outside;
Step 2, passes into boron trifluoride in the deionized water of reactor, makes boron trifluoride and deionized water generation complex reaction, obtained boron trifluoride two hydrate.
Preferably, in described step 2, while passing into boron trifluoride, utilize mechanical stirrer agitating deionized water.
Preferably, the mass ratio of described deionized water and boron triflouride gas is 1: 1.5 ~ 2.5.
Preferably, the mass ratio of described deionized water and boron triflouride gas is 1: 1.7 ~ 2.1.
Preferably, the temperature of described complex reaction controls at 0 ~ 45 DEG C.
Preferably, the temperature of described complex reaction controls at 15 ~ 35 DEG C.
Preferably, 5 ~ 12 hours reaction times of described complex reaction.
Preferably, 7 ~ 10 hours reaction times of described complex reaction.
The invention has the beneficial effects as follows: the preparation method of boron trifluoride two hydrate provided by the invention, adopt deionized water as medium, water vapor and boron triflouride gas generation complex reaction obtain boron trifluoride complex, i.e. boron trifluoride two hydrate, due to not with an organic solvent, with low cost and environmental protection; This complex reaction normal temperature or slightly relative superiority or inferiority carry out, reaction temperature and, reaction conditions be more prone to control, also safer.
Embodiment
In order to more clearly state the present invention, below in conjunction with specific embodiment, the present invention is further described.
Embodiment 1
In this embodiment, the production technique of boron trifluoride two hydrate comprises the following steps:
Step one, joins deionized water and is connected to prolong, mechanical stirrer, tetrafluoroethylene BF 3in the there-necked flask of ventpipe, there-necked flask is carried out cold cycle cooling;
Step 2, opens mechanical stirrer and stirs deionized water, and import boron triflouride gas and carry out complex reaction, reaction equation is: BF 3+ 2OH 2→ BF 32OH 2.Wherein, the mass ratio of deionized water and boron triflouride gas is 1: 1.5, and temperature controls at 45 DEG C, 7 hours reaction times, finally obtained boron trifluoride complex, i.e. boron trifluoride two hydrate BF 32OH 2.
Embodiment 2
In this embodiment, the production technique of boron trifluoride two hydrate comprises the following steps:
Step one, joins deionized water and is connected to prolong, mechanical stirrer, tetrafluoroethylene BF 3in the there-necked flask of ventpipe, there-necked flask is carried out cold cycle cooling;
Step 2, opens mechanical stirrer and stirs deionized water, and import boron triflouride gas and carry out complex reaction, reaction equation is: BF 3+ 2OH 2→ BF 32OH 2.Wherein, the mass ratio of deionized water and boron triflouride gas is 1: 1.7, and temperature controls at 0 DEG C, 5 hours reaction times, finally obtained boron trifluoride complex, i.e. boron trifluoride two hydrate BF 32OH 2.
Embodiment 3
In this embodiment, the production technique of boron trifluoride two hydrate comprises the following steps:
Step one, joins deionized water and is connected to prolong, mechanical stirrer, tetrafluoroethylene BF 3in the there-necked flask of ventpipe, there-necked flask is carried out cold cycle cooling;
Step 2, opens mechanical stirrer and stirs deionized water, and import boron triflouride gas and carry out complex reaction, reaction equation is: BF 3+ 2OH 2→ BF 32OH 2.Wherein, the mass ratio of deionized water and boron triflouride gas is 1: 2.5, and temperature controls at 15 DEG C, 12 hours reaction times, finally obtained boron trifluoride complex, i.e. boron trifluoride two hydrate BF 32OH 2.
Embodiment 4
In this embodiment, the production technique of boron trifluoride two hydrate comprises the following steps:
Step one, joins deionized water and is connected to prolong, mechanical stirrer, tetrafluoroethylene BF 3in the there-necked flask of ventpipe, there-necked flask is carried out cold cycle cooling;
Step 2, opens mechanical stirrer and stirs deionized water, and import boron triflouride gas and carry out complex reaction, reaction equation is: BF 3+ 2OH 2→ BF 32OH 2.Wherein, the mass ratio of deionized water and boron triflouride gas is 1: 2.1, and temperature controls at 35 DEG C, 10 hours reaction times, finally obtained boron trifluoride complex, i.e. boron trifluoride two hydrate BF 32OH 2.
Embodiment 5
In this embodiment, the production technique of boron trifluoride two hydrate comprises the following steps:
Step one, joins deionized water and is connected to prolong, mechanical stirrer, tetrafluoroethylene BF 3in the there-necked flask of ventpipe, there-necked flask is carried out cold cycle cooling;
Step 2, opens mechanical stirrer and stirs deionized water, and import boron triflouride gas and carry out complex reaction, reaction equation is: BF 3+ 2OH 2→ BF 32OH 2.Wherein, the mass ratio of deionized water and boron triflouride gas is 1: 2.2, and temperature controls at 30 DEG C, 8 hours reaction times, finally obtained boron trifluoride complex, i.e. boron trifluoride two hydrate BF 32OH 2.
From above-described embodiment, can confirm:
The preparation method of boron trifluoride two hydrate provided by the invention, water vapor and boron triflouride gas generation complex reaction obtain boron trifluoride complex, i.e. boron trifluoride two hydrate, due to not with an organic solvent, with low cost and environmental protection; Complex reaction normal temperature or slightly relative superiority or inferiority carry out, reaction temperature and, reaction conditions be more prone to control, also safer.
These are only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.

Claims (8)

1. a preparation method for boron trifluoride two hydrate, is characterized in that, comprise the following steps:
Step one, adds deionized water in the reactor, and cooling process is carried out in reactor outside;
Step 2, passes into boron trifluoride in the deionized water of reactor, makes boron trifluoride and deionized water generation complex reaction, obtained boron trifluoride two hydrate.
2. the preparation method of boron trifluoride two hydrate according to claim 1, is characterized in that, in described step 2, while passing into boron trifluoride, utilizes mechanical stirrer agitating deionized water.
3. the preparation method of boron trifluoride two hydrate according to claim 1, is characterized in that, the mass ratio of described deionized water and boron triflouride gas is 1: 1.5 ~ 2.5.
4. the preparation method of boron trifluoride two hydrate according to claim 3, is characterized in that, the mass ratio of described deionized water and boron triflouride gas is 1: 1.7 ~ 2.1.
5. the preparation method of boron trifluoride two hydrate according to claim 1, is characterized in that, the temperature of described complex reaction controls at 0 ~ 45 DEG C.
6. the preparation method of boron trifluoride two hydrate according to claim 5, is characterized in that, the temperature of described complex reaction controls at 15 ~ 35 DEG C.
7. the preparation method of boron trifluoride two hydrate according to claim 1, is characterized in that, 5 ~ 12 hours reaction times of described complex reaction.
8. the preparation method of boron trifluoride two hydrate according to claim 7, is characterized in that, 7 ~ 10 hours reaction times of described complex reaction.
CN201510907686.7A 2015-12-09 2015-12-09 Preparation method of boron trifluoride dihydrate Pending CN105314644A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110902963A (en) * 2019-12-10 2020-03-24 九江天赐高新材料有限公司 Treatment method of alkali-soluble polymer-containing wastewater

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1231214A (en) * 1997-12-08 1999-10-13 埃勒夫阿托化学有限公司 Preparation of boron trifluoride and sulfuric acid from boron trifluoride hydrate
CN102911195A (en) * 2012-10-31 2013-02-06 江峰 Preparation method of boron trifluoride tetrahydrofuran

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1231214A (en) * 1997-12-08 1999-10-13 埃勒夫阿托化学有限公司 Preparation of boron trifluoride and sulfuric acid from boron trifluoride hydrate
CN102911195A (en) * 2012-10-31 2013-02-06 江峰 Preparation method of boron trifluoride tetrahydrofuran

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
张卫江 等: ""三氟化硼纯化技术研究进展"", 《化工进展》 *
闫 华 等: ""三氟化硼和水反应的密度泛函理论研究"", 《化学学报》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110902963A (en) * 2019-12-10 2020-03-24 九江天赐高新材料有限公司 Treatment method of alkali-soluble polymer-containing wastewater

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