CN108101932A - A kind of butyl borate - Google Patents
A kind of butyl borate Download PDFInfo
- Publication number
- CN108101932A CN108101932A CN201711448264.3A CN201711448264A CN108101932A CN 108101932 A CN108101932 A CN 108101932A CN 201711448264 A CN201711448264 A CN 201711448264A CN 108101932 A CN108101932 A CN 108101932A
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- CN
- China
- Prior art keywords
- reaction
- butyl borate
- preparation process
- water
- present
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- 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.)
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- LGQXXHMEBUOXRP-UHFFFAOYSA-N tributyl borate Chemical compound CCCCOB(OCCCC)OCCCC LGQXXHMEBUOXRP-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000006243 chemical reaction Methods 0.000 claims abstract description 36
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000004327 boric acid Substances 0.000 claims abstract description 7
- 238000004821 distillation Methods 0.000 claims abstract description 6
- 238000010792 warming Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 3
- 238000002360 preparation method Methods 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 8
- 238000005485 electric heating Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 229910000831 Steel Inorganic materials 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 239000010959 steel Substances 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 abstract description 8
- 230000035484 reaction time Effects 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000010992 reflux Methods 0.000 abstract description 4
- 230000000630 rising effect Effects 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 238000005292 vacuum distillation Methods 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 230000032050 esterification Effects 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- -1 borate ester Chemical class 0.000 description 1
- NOXNXVPLDITALF-UHFFFAOYSA-N butoxyboronic acid Chemical class CCCCOB(O)O NOXNXVPLDITALF-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000003254 gasoline additive Substances 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000004094 surface-active agent Substances 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
- C07F5/04—Esters of boric acids
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
Abstract
The present invention relates to chemical fields, disclose a kind of butyl borate, are made by the steps：(1) vacuum is pumped into 2300 2700kg n-butanols in 2500 3500L reaction kettles；(2) 400 410kg boric acid are put by manhole, starts stirring, be warming up to 115 120 DEG C, back flow reaction, with the water of time-division dereaction generation；(3) when anhydrous generation, extra n-butanol is evaporated off；(4) reaction solution is pressed into distillation still, is evaporated under reduced pressure, obtains finally required butyl borate.Advantages of the present invention is：(1) simple production process, easy to operate；(2) reacted using temperature rising reflux, with the water of time-division dereaction generation in reaction process, accelerate reaction rate；(3) compared with conventional heating mode, the reaction time is shortened, improves butyl borate yield and purity.
Description
Technical field
The present invention relates to chemical field more particularly to a kind of butyl borates.
Background technology
Butyl borate is the intermediate for preparing hydroboron, available for synthesis semiconductor boron diffusion source, fireproof agent, is glued
Mixture and anhydrous systems drier, in addition, can also make polymeric additive, gasoline additive, bactericidal agent, fire retardant, automobile system
Hydrodynamic and special surfactant use, and application range is very extensive.
At present, the synthesis of borate ester product is mainly obtained using boric acid and alcohol as raw material direct esterification, traditional heating item
Reaction needs 4-5h under part；Reaction temperature needed for most of esterifications is still using traditional heating method, and the reaction time is long, yield
It is relatively low, and the purity of final products is nor very high.
Therefore, be badly in need of at present it is a kind of prepare that the reaction time is short, yield is high, and the butyl borate product that finished product purity is high.
The content of the invention
Prepare that the reaction time is short, yield is high it is an object of the invention to overcome the deficiencies of the prior art and provide a kind of, and
The high butyl borate of finished product purity.
The present invention is achieved by the following technical solutions：A kind of butyl borate, is made by the steps：
(1) vacuum is pumped into 2300-2700kg n-butanols in 2500-3500L reaction kettles；
(2) 400-410kg boric acid is put by manhole, starts stirring, be warming up to 115-120 DEG C, back flow reaction, the same to time-division
The water of dereaction generation；
(3) when anhydrous generation, extra n-butanol is evaporated off；
(4) reaction solution is pressed into distillation still, is evaporated under reduced pressure, obtains finally required butyl borate.
One of preferred embodiment as the present invention, reaction kettle is stainless steel electric heating reacting kettle in the preparation process (1).
One of preferred embodiment as the present invention, in the pressure of (- 0.07 5)-(- 0.065) MPa in the preparation process (1)
Vacuum is pumped into n-butanol under power.
One of preferred embodiment as the present invention, the preparation process (2) is middle to use blender to the mixing in reaction kettle
Solution is stirred.
One of preferred embodiment as the present invention, mixing speed is 60-70rpm/min in the preparation process (2).
One of preferred embodiment as the present invention, middle use of the preparation process (2) divide water operation point to remove n-butanol and boron
The water generated in sour reaction process.
One of preferred embodiment as the present invention, in (- 0.1)-(- 0.09) MPa, 125-135 in the preparation process (4)
It is evaporated under reduced pressure under conditions of DEG C.
The present invention compared with prior art the advantages of be：The simple production process, easy to operate of the present invention, using heating up back
Stream reacts, and with the water of time-division dereaction generation in reaction process, accelerates reaction rate；It is compared with conventional heating mode, contracting
In the short reaction time, improve butyl borate yield and purity.
Description of the drawings
Fig. 1 is the preparation flow figure of the butyl borate in embodiment 1-3.
Specific embodiment
It elaborates below to the embodiment of the present invention, the present embodiment is carried out lower based on the technical solution of the present invention
Implement, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following implementation
Example.
Embodiment 1
A kind of butyl borate of the present embodiment, as shown in Figure 1, being made by the steps：
(1) -0.075MPa vacuum is pumped into 2300kg n-butanols in 2500L stainless steel electric heating reacting kettles；
(2) 400kg boric acid is put by manhole, starts blender, mixed solution is stirred with the speed of 60rpm/min
It mixes, is warming up to 115 DEG C, back flow reaction, while using the water for dividing water operation point dereaction generation；
(3) when anhydrous generation, extra n-butanol is evaporated off；
(4) reaction solution is pressed into distillation still, in -0.1MPa, 125 DEG C of condition vacuum distillation finally obtains index parameter
Butyl borate as shown in Table 1, reaction equation are as follows：
The butyl borate index parameter of 1 embodiment 1 of table
| Sequence number | Index | Numerical value |
| 1 | Appearance | Colorless clear liquid |
| 2 | Purity | ＞ 99% |
It is the simple production process of the present embodiment, easy to operate；It is reacted using temperature rising reflux, is gone instead with the time-division in reaction process
The water that should be generated, accelerates reaction rate；Compared with conventional heating mode, the reaction time is shortened, improves butyl borate
Yield and purity.
Embodiment 2
A kind of butyl borate of the present embodiment, as shown in Figure 1, being made by the steps：
(1) -0.065MPa vacuum is pumped into 2700kg n-butanols in 3500L stainless steel electric heating reacting kettles；
(2) 410kg boric acid is put by manhole, starts blender, mixed solution is stirred with the speed of 70rpm/min
It mixes, is warming up to 120 DEG C, back flow reaction, while using the water for dividing water operation point dereaction generation；
(3) when anhydrous generation, extra n-butanol is evaporated off；
(4) reaction solution is pressed into distillation still, in -0.09MPa, 135 DEG C of condition vacuum distillation finally obtains index parameter
Butyl borate as shown in Table 2, reaction equation are as follows：
The butyl borate index parameter of 2 embodiment 2 of table
| Sequence number | Index | Numerical value |
| 1 | Appearance | Colorless clear liquid |
| 2 | Purity | ＞ 99% |
It is the simple production process of the present embodiment, easy to operate；It is reacted using temperature rising reflux, is gone instead with the time-division in reaction process
The water that should be generated, accelerates reaction rate；Compared with conventional heating mode, the reaction time is shortened, improves butyl borate
Yield and purity.
Embodiment 3
A kind of butyl borate of the present embodiment, as shown in Figure 1, being made by the steps：
(1) -0.07MPa vacuum is pumped into 2500kg n-butanols in 3000L stainless steel electric heating reacting kettles；
(2) 405kg boric acid is put by manhole, starts blender, mixed solution is stirred with the speed of 65rpm/min
It mixes, is warming up to 118 DEG C, back flow reaction, while using the water for dividing water operation point dereaction generation；
(3) when anhydrous generation, extra n-butanol is evaporated off；
(4) reaction solution is pressed into distillation still, in -0.095MPa, 130 DEG C of condition vacuum distillation finally obtains index ginseng
Number butyl borate as shown in table 3, reaction equation are as follows：
The butyl borate index parameter of 3 embodiment 3 of table
| Sequence number | Index | Numerical value |
| 1 | Appearance | Colorless clear liquid |
| 2 | Purity | ＞ 99% |
It is the simple production process of the present embodiment, easy to operate；It is reacted using temperature rising reflux, is gone instead with the time-division in reaction process
The water that should be generated, accelerates reaction rate；Compared with conventional heating mode, the reaction time is shortened, improves butyl borate
Yield and purity.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should all be included in the protection scope of the present invention.
Claims (7)
1. a kind of butyl borate, which is characterized in that be made by the steps：
(1) vacuum is pumped into 2300-2700kg n-butanols in 2500-3500L reaction kettles；
(2) 400-410kg boric acid is put by manhole, starts stirring, be warming up to 115-120 DEG C, back flow reaction is gone instead with the time-division
The water that should be generated；
(3) when anhydrous generation, extra n-butanol is evaporated off；
(4) reaction solution is pressed into distillation still, is evaporated under reduced pressure, obtains finally required butyl borate.
2. butyl borate according to claim 1, which is characterized in that reaction kettle is stainless in the preparation process (1)
Steel electric heating reacting kettle.
3. butyl borate according to claim 1, which is characterized in that in the preparation process (1) (- 0.07 5)-
The vacuum under pressure of (- 0.065) MPa is pumped into n-butanol.
4. butyl borate according to claim 1, which is characterized in that blender pair is used in the preparation process (2)
Mixed solution in reaction kettle is stirred.
5. butyl borate according to claim 1, which is characterized in that mixing speed is 60- in the preparation process (2)
70rpm/min。
6. butyl borate according to claim 1, which is characterized in that used in the preparation process (2) and water is divided to operate
Divide the water for removing n-butanol and being generated during acid reaction.
7. butyl borate according to claim 1, which is characterized in that in the preparation process (4) (- 0.1)-(-
0.09) it is evaporated under reduced pressure under conditions of MPa, 125-135 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711448264.3A CN108101932A (en) | 2017-12-27 | 2017-12-27 | A kind of butyl borate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711448264.3A CN108101932A (en) | 2017-12-27 | 2017-12-27 | A kind of butyl borate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108101932A true CN108101932A (en) | 2018-06-01 |
Family
ID=62213963
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711448264.3A Withdrawn CN108101932A (en) | 2017-12-27 | 2017-12-27 | A kind of butyl borate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108101932A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116253757A (en) * | 2023-01-17 | 2023-06-13 | 大连爱柏斯化工股份有限公司 | Tributyl borate formula and preparation method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102766152A (en) * | 2012-07-04 | 2012-11-07 | 梁嘉鸣 | Method for preparing tributyl borate by utilizing reactant n-butyl alcohol as water-carrying agent |
-
2017
- 2017-12-27 CN CN201711448264.3A patent/CN108101932A/en not_active Withdrawn
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102766152A (en) * | 2012-07-04 | 2012-11-07 | 梁嘉鸣 | Method for preparing tributyl borate by utilizing reactant n-butyl alcohol as water-carrying agent |
Non-Patent Citations (2)
| Title |
|---|
| 张吉初 等: "硼酸三丁酯的合成", 《化学工业与工程》 * |
| 梁兵 等: "金属-橡胶粘合促进剂硼酰化钴的制备及性能", 《沈阳化工大学学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116253757A (en) * | 2023-01-17 | 2023-06-13 | 大连爱柏斯化工股份有限公司 | Tributyl borate formula and preparation method |
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| PB01 | Publication | ||
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Application publication date: 20180601 |