CN111423461A - Hydrolysis resistance method of boron trifluoride methyl ether complex - Google Patents
Hydrolysis resistance method of boron trifluoride methyl ether complex Download PDFInfo
- Publication number
- CN111423461A CN111423461A CN202010248384.4A CN202010248384A CN111423461A CN 111423461 A CN111423461 A CN 111423461A CN 202010248384 A CN202010248384 A CN 202010248384A CN 111423461 A CN111423461 A CN 111423461A
- Authority
- CN
- China
- Prior art keywords
- complex
- dehydrating agent
- rectification
- methyl ether
- boron trifluoride
- 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
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- WTEOIRVLGSZEPR-UHFFFAOYSA-N boron trifluoride Chemical compound FB(F)F WTEOIRVLGSZEPR-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 30
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 229910015900 BF3 Inorganic materials 0.000 title claims abstract description 26
- 230000007062 hydrolysis Effects 0.000 title claims description 11
- 238000006460 hydrolysis reaction Methods 0.000 title claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000012024 dehydrating agents Substances 0.000 claims description 35
- DMEGYFMYUHOHGS-UHFFFAOYSA-N heptamethylene Natural products C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 7
- RGSFGYAAUTVSQA-UHFFFAOYSA-N pentamethylene Natural products C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 claims description 6
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 4
- 125000001511 cyclopentyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C1([H])[H] 0.000 claims description 2
- 238000004064 recycling Methods 0.000 claims description 2
- 230000000655 anti-hydrolysis Effects 0.000 abstract description 3
- 239000002351 wastewater Substances 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 230000018044 dehydration Effects 0.000 description 4
- 238000006297 dehydration reaction Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- UHZYTMXLRWXGPK-UHFFFAOYSA-N phosphorus pentachloride Chemical compound ClP(Cl)(Cl)(Cl)Cl UHZYTMXLRWXGPK-UHFFFAOYSA-N 0.000 description 2
- RILZRCJGXSFXNE-UHFFFAOYSA-N 2-[4-(trifluoromethoxy)phenyl]ethanol Chemical compound OCCC1=CC=C(OC(F)(F)F)C=C1 RILZRCJGXSFXNE-UHFFFAOYSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-BJUDXGSMSA-N Boron-10 Chemical compound [10B] ZOXJGFHDIHLPTG-BJUDXGSMSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/02—Boron compounds
- C07F5/022—Boron compounds without C-boron linkages
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the field of chemical synthesis and separation, and particularly relates to an anti-hydrolysis method of a boron trifluoride methyl ether complex. The invention removes the water in the complex in real time in the rectification process and takes the water out of the rectification system, thereby protecting the rectification equipment while generating no wastewater. The method has the advantages that the complex can be effectively inhibited from being hydrolyzed under the temperature condition in the rectification process, water is not required to be removed before the complex enters the rectification tower, and the secondary environmental problem is avoided.
Description
Technical Field
The invention belongs to the field of chemical synthesis and separation, and particularly relates to an anti-hydrolysis method of a boron trifluoride methyl ether complex.
Background
The method for preparing the boron-10 acid by adopting the dimethyl ether complex requires that the complex is dehydrated before entering a tower and the water in the complex is removed by phosphorus pentachloride. This dehydration method does not completely remove the water, the water remaining in the complex is very harmful, and the complex is hydrolyzed under the process conditions of the rectification process and reaction water is regenerated, thus causing a dead cycle of endless hydrolysis and decomposing most of the complex.
Phosphorus pentachloride dehydration can generate wastewater containing chlorine and phosphorus, the harm of the chlorine and the phosphorus is not easy to eliminate, and a dehydrated complex can carry the chlorine and the phosphorus to corrode rectification equipment.
Disclosure of Invention
Aiming at the existing problems, the invention provides an anti-hydrolysis method of a boron trifluoride methyl ether complex, which aims to remove water in the complex in real time in the rectification process and take water out of a rectification system, so that no waste water is generated and rectification equipment is protected.
The hydrolysis resistance method of the boron trifluoride methyl ether complex is carried out according to the following steps:
adding a boron trifluoride methyl ether complex which is not dehydrated in advance into a rectification system, adding a dehydrating agent into a tower kettle of a rectification tower, fully contacting the boron trifluoride methyl ether complex with the dehydrating agent in the rectification process, continuously absorbing moisture in the complex by the dehydrating agent, and continuously taking the moisture out of the rectification system by the dehydrating agent, wherein the moisture content of the complex is less than 50 ppm.
Wherein the dehydrating agent is cyclopentane, cyclohexane or cycloheptane.
The addition amount of the dehydrating agent is 10-15 times of the moisture content in the complex.
After leaving the rectification system, the dehydrating agent is kept stand in a separator to be naturally separated from water, and the solvent returns to the tower to be recycled.
Compared with the prior art, the invention has the characteristics and beneficial effects that:
the dehydrating agent of the invention is cyclopentane, cyclohexane and cycloheptane; the dehydration principle is that water is carried by azeotropic boiling in the tower, the water is naturally separated after leaving the tower and stands in a separator, and the solvent is returned to the tower for recycling.
The method has the advantages that the complex can be effectively inhibited from being hydrolyzed under the temperature condition in the rectification process, water is not required to be removed before the complex enters the rectification tower, and the secondary environmental problem is avoided.
The invention can dehydrate on line in real time in the rectification process, can control the water content of the material in the key link in the system to be less than 50ppm, and effectively inhibits the hydrolysis of boron trifluoride methyl ether complex.
The method has obvious dehydration effect, eliminates the problem of tower blockage caused by boric acid crystallization due to hydrolysis of the boron trifluoride methyl ether complex, and effectively avoids the problem of corrosion of equipment caused by fluoroboric acid and hydrofluoric acid generated by hydrolysis of the boron trifluoride methyl ether complex.
Detailed Description
The following description is of preferred embodiments of the present invention, and it should be understood that the preferred embodiments described herein are for purposes of illustration only and are not intended to limit the invention.
Example 1:
the method for resisting hydrolysis of boron trifluoride methyl ether complex of this example was carried out according to the following steps:
adding a boron trifluoride methyl ether complex which is not dehydrated in advance into a rectification system, adding a dehydrating agent cyclopentane into a tower kettle of a rectification tower, adding the dehydrating agent according to the amount of 10 times of the moisture content in the complex, fully contacting the boron trifluoride methyl ether complex with the dehydrating agent in the rectification process, continuously absorbing the moisture in the complex by the dehydrating agent, and continuously taking the moisture out of the rectification system by the dehydrating agent, detecting the water content of the boron trifluoride methyl ether complex by a trace moisture analyzer (Karl Fischer's reagent), and detecting the material moisture content of the complex to be less than 50 ppm.
After the dehydrating agent leaves the rectification system, the dehydrating agent is kept stand in a separator to be naturally separated from water, and the solvent returns to the tower to be recycled.
Example 2:
the method for resisting hydrolysis of boron trifluoride methyl ether complex of this example was carried out according to the following steps:
adding a boron trifluoride methyl ether complex which is not dehydrated in advance into a rectification system, adding a dehydrating agent cyclohexane into a tower kettle of a rectification tower, wherein the adding amount of the dehydrating agent is 15 times of the moisture content in the complex, the boron trifluoride methyl ether complex is fully contacted with the dehydrating agent in the rectification process, the moisture in the complex is continuously absorbed by the dehydrating agent and is continuously taken out of the rectification system by the dehydrating agent, the moisture content of the boron trifluoride methyl ether complex is detected by a trace moisture analyzer (Karl Fischer's reagent), and the moisture content of the material of the complex is detected to be less than 50 ppm.
After the dehydrating agent leaves the rectification system, the dehydrating agent is kept stand in a separator to be naturally separated from water, and the solvent returns to the tower to be recycled.
Example 3:
the method for resisting hydrolysis of boron trifluoride methyl ether complex of this example was carried out according to the following steps:
adding boron trifluoride methyl ether complex which is not dehydrated in advance into a rectification system, adding dehydrating agent cycloheptane into a tower kettle of a rectification tower, adding the dehydrating agent according to the amount which is 12 times of the moisture content in the complex, fully contacting the boron trifluoride methyl ether complex with the dehydrating agent in the rectification process, continuously absorbing the moisture in the complex by the dehydrating agent and continuously taking the moisture out of the rectification system by the dehydrating agent, detecting the moisture content of the boron trifluoride methyl ether complex by a trace moisture analyzer (Karl Fischer's reagent), and detecting the material moisture content of the complex to be less than 50 ppm.
After the dehydrating agent leaves the rectification system, the dehydrating agent is kept stand in a separator to be naturally separated from water, and the solvent returns to the tower to be recycled.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. A method for resisting hydrolysis of boron trifluoride methyl ether complex is characterized by comprising the following steps:
adding a boron trifluoride methyl ether complex which is not dehydrated in advance into a rectification system, adding a dehydrating agent into a tower kettle of a rectification tower, fully contacting the boron trifluoride methyl ether complex with the dehydrating agent in the rectification process, continuously absorbing moisture in the complex by the dehydrating agent, and continuously taking the moisture out of the rectification system by the dehydrating agent, wherein the moisture content of the complex is less than 50 ppm.
2. The method of claim 1, wherein the dehydrating agent is cyclopentane, cyclohexane or cycloheptane.
3. The method of claim 1, wherein the dehydrating agent is added in an amount of 10 to 15 times the water content of the complex.
4. The method of claim 1, wherein the dehydrating solvent is left in a separator after leaving the rectification system, standing and naturally separating water, and the solvent is returned to the column for recycling.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010248384.4A CN111423461A (en) | 2020-04-01 | 2020-04-01 | Hydrolysis resistance method of boron trifluoride methyl ether complex |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010248384.4A CN111423461A (en) | 2020-04-01 | 2020-04-01 | Hydrolysis resistance method of boron trifluoride methyl ether complex |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111423461A true CN111423461A (en) | 2020-07-17 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010248384.4A Pending CN111423461A (en) | 2020-04-01 | 2020-04-01 | Hydrolysis resistance method of boron trifluoride methyl ether complex |
Country Status (1)
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|---|---|
| CN (1) | CN111423461A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB736984A (en) * | 1951-11-28 | 1955-09-14 | Celanese Corp | Improvements in or relating to the dehydration of liquids by azeotropic distillation |
| WO2008140957A2 (en) * | 2007-05-08 | 2008-11-20 | Huntsman International Llc | Separation of n,n,n'-trimethylbisaminoethylether from mixtures comprising tertiary amines or tertiary aminoalkylethrs |
| CN104209003A (en) * | 2014-08-16 | 2014-12-17 | 刘小秦 | Industrial production method for separating boron isotope product based on methyl-phenoxide-boron trifluoride complex |
| CN109534940A (en) * | 2017-09-22 | 2019-03-29 | 中昊晨光化工研究院有限公司 | A kind of depth drying water-eliminating method for dipentene |
| CN110698337A (en) * | 2019-08-28 | 2020-01-17 | 派尔科化工材料（启东）有限公司 | Production method of electronic grade cyclopentanone |
| CN111410205A (en) * | 2020-03-30 | 2020-07-14 | 辽宁鸿昊化学工业股份有限公司 | Preparation method of high-abundance and high-purity nuclear-grade boron-10 acid |
-
2020
- 2020-04-01 CN CN202010248384.4A patent/CN111423461A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB736984A (en) * | 1951-11-28 | 1955-09-14 | Celanese Corp | Improvements in or relating to the dehydration of liquids by azeotropic distillation |
| WO2008140957A2 (en) * | 2007-05-08 | 2008-11-20 | Huntsman International Llc | Separation of n,n,n'-trimethylbisaminoethylether from mixtures comprising tertiary amines or tertiary aminoalkylethrs |
| CN104209003A (en) * | 2014-08-16 | 2014-12-17 | 刘小秦 | Industrial production method for separating boron isotope product based on methyl-phenoxide-boron trifluoride complex |
| CN109534940A (en) * | 2017-09-22 | 2019-03-29 | 中昊晨光化工研究院有限公司 | A kind of depth drying water-eliminating method for dipentene |
| CN110698337A (en) * | 2019-08-28 | 2020-01-17 | 派尔科化工材料（启东）有限公司 | Production method of electronic grade cyclopentanone |
| CN111410205A (en) * | 2020-03-30 | 2020-07-14 | 辽宁鸿昊化学工业股份有限公司 | Preparation method of high-abundance and high-purity nuclear-grade boron-10 acid |
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