CN106397469A - Continuous cycle preparation method of trimethyl borate - Google Patents
Continuous cycle preparation method of trimethyl borate Download PDFInfo
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- CN106397469A CN106397469A CN201510473201.8A CN201510473201A CN106397469A CN 106397469 A CN106397469 A CN 106397469A CN 201510473201 A CN201510473201 A CN 201510473201A CN 106397469 A CN106397469 A CN 106397469A
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- methyl borate
- methanol
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Abstract
The invention discloses a continuous cycle preparation method of trimethyl borate. Methanol and boric acid are added into a reactor to be subjected to a preliminary reaction, the preliminary reaction product enters a coarse steaming kettle to be evaporated and then enters a reaction rectifying tower to be subjected to rectification to obtain an azeotrope of trimethyl borate and methanol, and a salt-added solvent and the azeotrope are respectively added into an extraction rectification tower, the set temperature and the flow rate are controlled, and salt-adding extraction rectification is carried out, the tower bottom product is subjected to solvent recovery by a solvent recovery tower, and then the solvent is circulated into the extraction rectification tower for use. The method has the advantages of being low in equipment investment and energy consumption, the separation efficiency can be improved, the good technical effect is achieved, the product yield is high, the purity is high, the solvent can be recycled, and the practicability is good.
Description
Technical field
The present invention relates to Organic substance Preparation equipment technical field is and in particular to a kind of continuous circulation process of preparing of methyl borate..
Background technology
The continuous circulation process of preparing of existing methyl borate. normally only is used in conjunction to prepare using reactor and rectifying column, this device is final to obtain the azeotropic mixture being methyl borate. with methanol, need just to obtain end-product methyl borate. after separating, do not enable the recycling use of solvent, therefore can't fully meet use demand.
Content of the invention
Goal of the invention：For the deficiencies in the prior art, it is an object of the invention to provide a kind of continuous circulation process of preparing of methyl borate., have that equipment investment is low, good separating effect, the features such as recycling.
Technical scheme：In order to realize foregoing invention purpose, the technical solution used in the present invention is as follows：
Methanol and boric acid are added in reactor, carry out initial reaction, it is evaporated subsequently into crude steam kettle, subsequently enter reactive distillation column and carry out rectification, obtain the azeotropic mixture of methyl borate. and methanol, salt adding solvent and azeotropic mixture are separately added into extractive distillation column, control design temperature and flow, carry out extractive distillation with salt, tower bottom product is passed through solvent recovery tower and carries out solvent recovery, then circulation is passed through extractive distillation column and uses.
Described solvent recovery tower is communicated with Salt Addition Extraction Refinery Tower by solvent circulation line.
Described reactor sets feed(raw material)inlet.
Beneficial effect：Compared with prior art, the continuous circulation process of preparing of the methyl borate. of the present invention, equipment investment is low and the low advantage of energy consumption, separation efficiency can be improved, achieve preferable technique effect, efficiency of pcr product is high, purity is high, and solvent can recycle, and has good practicality.
Brief description
Fig. 1 is the structural representation of the continuous circulation preparation technology device of methyl borate..
Specific embodiment
With reference to specific embodiment, the present invention is described further.
As shown in Figure 1, the continuous circulation preparation technology device of methyl borate., including reactor 1, crude steam kettle 2, reactive distillation column 3, Salt Addition Extraction Refinery Tower 4 and solvent recovery tower 5, reactor 1 sets feed(raw material)inlet, reactor 1 is communicated with crude steam kettle 2 by pipeline, crude steam kettle 2 is communicated with reactive distillation column 3 by pipeline, reactive distillation column 3 is communicated with Salt Addition Extraction Refinery Tower 4 by pipeline, Salt Addition Extraction Refinery Tower 4 is communicated with solvent recovery tower 5 by pipeline, and solvent recovery tower 5 is communicated with Salt Addition Extraction Refinery Tower 4 by solvent circulation line.
The continuous circulation preparation method of methyl borate., methanol and boric acid are added in reactor 1, carry out initial reaction, be evaporated subsequently into crude steam kettle 2, subsequently enter reactive distillation column 3 and carry out rectification, obtain the azeotropic mixture of methyl borate. and methanol, salt adding solvent and azeotropic mixture are separately added into extractive distillation column 4, control design temperature and flow, carry out extractive distillation with salt, tower bottom product is passed through solvent recovery tower 5 and carries out solvent recovery, and then circulation is passed through extractive distillation column 4 and uses.
The continuous circulation process of preparing of this methyl borate., equipment investment is low and the low advantage of energy consumption, can improve separation efficiency, achieve preferable technique effect.
Claims (3)
1. a kind of methyl borate. continuous circulation process of preparing it is characterised in that：Methanol and boric acid are added in reactor, carry out initial reaction, it is evaporated subsequently into crude steam kettle, subsequently enter reactive distillation column and carry out rectification, obtain the azeotropic mixture of methyl borate. and methanol, salt adding solvent and azeotropic mixture are separately added into extractive distillation column, control design temperature and flow, carry out extractive distillation with salt, tower bottom product is passed through solvent recovery tower and carries out solvent recovery, then circulation is passed through extractive distillation column and uses.
2. the continuous circulation process of preparing of methyl borate. according to claim 1 is it is characterised in that described solvent recovery tower is communicated with Salt Addition Extraction Refinery Tower by solvent circulation line.
3. the continuous circulation process of preparing of methyl borate. according to claim 1 is it is characterised in that set feed(raw material)inlet on described reactor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510473201.8A CN106397469A (en) | 2015-08-05 | 2015-08-05 | Continuous cycle preparation method of trimethyl borate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510473201.8A CN106397469A (en) | 2015-08-05 | 2015-08-05 | Continuous cycle preparation method of trimethyl borate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106397469A true CN106397469A (en) | 2017-02-15 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510473201.8A Pending CN106397469A (en) | 2015-08-05 | 2015-08-05 | Continuous cycle preparation method of trimethyl borate |
Country Status (1)
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| CN (1) | CN106397469A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111233912A (en) * | 2019-12-24 | 2020-06-05 | 大连理工大学 | Method for semi-continuously synthesizing trimethyl borate-methanol azeotrope |
| CN116041379A (en) * | 2023-02-27 | 2023-05-02 | 贵州威顿晶磷电子材料股份有限公司 | Environment-friendly preparation equipment and method for electronic grade trimethyl borate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102816178A (en) * | 2012-09-14 | 2012-12-12 | 南通鸿志化工有限公司 | Method and special device for separating trimethyl borate from carbinol mixture |
| CN103833780A (en) * | 2014-03-26 | 2014-06-04 | 天津普莱化工技术有限公司 | Novel process method for preparing trimethyl borate through continuous reactive distillation |
-
2015
- 2015-08-05 CN CN201510473201.8A patent/CN106397469A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102816178A (en) * | 2012-09-14 | 2012-12-12 | 南通鸿志化工有限公司 | Method and special device for separating trimethyl borate from carbinol mixture |
| CN103833780A (en) * | 2014-03-26 | 2014-06-04 | 天津普莱化工技术有限公司 | Novel process method for preparing trimethyl borate through continuous reactive distillation |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111233912A (en) * | 2019-12-24 | 2020-06-05 | 大连理工大学 | Method for semi-continuously synthesizing trimethyl borate-methanol azeotrope |
| CN116041379A (en) * | 2023-02-27 | 2023-05-02 | 贵州威顿晶磷电子材料股份有限公司 | Environment-friendly preparation equipment and method for electronic grade trimethyl borate |
| CN116041379B (en) * | 2023-02-27 | 2023-09-26 | 贵州威顿晶磷电子材料股份有限公司 | Environment-friendly manufacturing method and matched manufacturing equipment for electronic grade trimethyl borate |
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170215 |
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| RJ01 | Rejection of invention patent application after publication |