CN101463041B - Production method of high-purity triisopropyl borate ester - Google Patents
Production method of high-purity triisopropyl borate ester Download PDFInfo
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- CN101463041B CN101463041B CN2007101797162A CN200710179716A CN101463041B CN 101463041 B CN101463041 B CN 101463041B CN 2007101797162 A CN2007101797162 A CN 2007101797162A CN 200710179716 A CN200710179716 A CN 200710179716A CN 101463041 B CN101463041 B CN 101463041B
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- borate ester
- triisopropyl borate
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- virahol
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Abstract
The invention discloses a production method of high-purity triisopropyl borate ester. The production method comprises the following steps: boric acid and isopropyl alcohol are taken as raw materials, and a mixture of benzene, toluene and cyclohexane is taken as a constant boiling agent, the materials react and are rectified in a tank reactor, then are subject to binary batch rectification to separate water from the constant boiling agent, and then subject to ternary batch rectification to separate out the isopropyl alcohol. In the production method, a reaction rectification technology plus the constant boiling agent is adopted for separating byproduct water from a reaction system, which improves the conversion ratio of the reaction and solves the disadvantages of inconvenient operation of a calcium hydride dehydrant, difficult solid waste treatment and high operation risk; and a novel batch rectification technology with a top tower storage tank is adopted for refining a crude product, which can obtain the high-purity triisopropyl borate ester with the content more than 99.0% and ensures that recovered isopropyl alcohol can be recycled.
Description
Technical field
The invention provides a kind of production method of high-purity triisopropyl borate ester, especially a kind of production method of high-purity triisopropyl borate ester.
Background technology
Triisopropyl borate ester is a kind of extremely important organic boron fine chemical material, mainly as organic intermediate and the medicine intermediate of producing coupling agent, in addition, also as the stablizer in the antifriction additive of lubricating oil, rubber one metlbond promotor, the polymkeric substance etc., production method mainly adopts boric acid or boric anhydride with pure esterification, use hydrolith as dewatering agent, product line purity is generally 94～96%.
Use hydrolith as dewatering agent in the existing technology, can produce calcium hydroxide precipitation and hydrogen, its shortcoming is inconvenient operation, useless admittedly difficult treatment, operational danger is big, product purity is not high.
Summary of the invention
The purpose of this invention is to provide a kind of production method of high-purity triisopropyl borate ester, it is made up of following steps:
A: with boric acid and Virahol is the tank reactor that raw material joins the band rectifying tower;
B: the mixture with benzene, toluene, hexanaphthene is a nonvariant boiling reagent, carries out reactive distillation in the tank reactor of band rectifying tower, and cat head is told water, and the tower still obtains the crude product of boronic acid containing three isopropyl esters;
C: the crude product to triisopropyl borate ester in the rectifying tower of band cat head storage tank carries out batch fractionating;
D: separate interim fraction, continue simple distillation and obtain triisopropyl borate ester;
E: in rectifying tower the water of telling among the step b is carried out the sequence of constant boiling and rectification at intermittence, the Virahol of recovery and nonvariant boiling reagent join among the step b.
The boric acid that adds among the described step a and the ratio of Virahol are 1: 3.5～6.
The ratio of described step b mesoboric acid and nonvariant boiling reagent is 1: 1.5～2.6.
The temperature of reactive distillation is 82 ℃～86 ℃ among the described step b.
Among the described step b in the nonvariant boiling reagent ratio of each component be benzene: toluene: hexanaphthene equals 3: 1: 1.
Described step c or e intermittence sequence of constant boiling and rectification for carrying out the binary batch fractionating earlier, divide dried up and nonvariant boiling reagent, carry out again ternary intermittently sequence of constant boiling and rectification isolate Virahol.
Advantage of the present invention is to adopt the reaction rectification technique that adds nonvariant boiling reagent to isolate water byproduct from reaction system, improve the transformation efficiency of reaction, inconvenient, the useless admittedly difficult treatment of solution hydrolith dewatering agent operation, the shortcoming that operational danger is big, adopt the refining crude product of novel intermittent distillation technology of band cat head storage tank, can obtain content greater than 99.0% high-purity triisopropyl borate ester, the Virahol and the nonvariant boiling reagent of recovery can be recycled; But if with the hexanaphthene to be nonvariant boiling reagent production pharmaceutical grade (not containing benzene) high-purity triisopropyl borate ester separately.
Description of drawings
Figure is a FB(flow block) of the present invention.
Embodiment
Further specify the present invention below by embodiment:
Embodiment 1:
As shown in the figure, get boric acid 125kg, Virahol 500kg, hexanaphthene 60kg, add 1m from charging opening 1
3In the reactor 2, rectifying tower 3 diameter 0.4m, wire mesh packing, height 4m, the volume of head tower storage tank 4 is 60L, and reactor 2 is heated, be warmed to 80 ℃, carry out the rectifying of binary gap earlier, carry out the thick product that ternary gap rectifying separation goes out Virahol, nonvariant boiling reagent and triisopropyl borate ester again.
Virahol, nonvariant boiling reagent are sent to through separator 5 and continue to participate in rectifying in the rectifying tower 3, the thick product of triisopropyl borate ester enters receiving tank 6 after separator 5 separates, again the thick product of receiving tank 6 mesoboric acids three isopropyl esters is proceeded simple distillation, can obtain 157kg triisopropyl borate ester product, by analysis, its content is 99.5%, and the one way yield is 74.7%, the cut that reclaims is Virahol and nonvariant boiling reagent, and omnidistance total recovery is 92.6%.
Embodiment 2:
As shown in the figure, get boric acid 300kg, Virahol 1000kg, hexanaphthene 150kg, add 3m from charging opening 1
3In the reactor 2, rectifying tower 3 diameter 0.8m, wire mesh packing, height 5m, the volume of head tower storage tank 4 is 120L, and reactor 2 is heated, be warmed to 80 ℃, carry out the rectifying of binary gap earlier, carry out the thick product that ternary gap rectifying separation goes out Virahol, nonvariant boiling reagent and triisopropyl borate ester again.
Virahol, nonvariant boiling reagent are sent to through separator 5 and continue to participate in rectifying in the rectifying tower 3, the thick product of triisopropyl borate ester enters receiving tank 6 after separator 5 separates, again the thick product of receiving tank 6 mesoboric acids three isopropyl esters is proceeded simple distillation, can obtain 370kg triisopropyl borate ester product, by analysis, its content is 99.4%, and the one way yield is 74.1%, the cut that reclaims is Virahol and nonvariant boiling reagent, and omnidistance total recovery is 92.3%.
Claims (6)
1. the production method of a high-purity triisopropyl borate ester is a raw material with boric acid and Virahol, and described high-purity triisopropyl borate ester is meant content greater than 99.0% triisopropyl borate ester, and it is characterized in that: it may further comprise the steps
A: with boric acid and Virahol is the tank reactor that raw material joins the band rectifying tower;
B: the mixture with benzene, toluene, hexanaphthene is a nonvariant boiling reagent, carries out reactive distillation in the tank reactor of band rectifying tower, and cat head is told water, and the tower still obtains the crude product of boronic acid containing three isopropyl esters;
C: the crude product to triisopropyl borate ester in the rectifying tower of band cat head storage tank carries out batch fractionating;
D: separate interim fraction, continue simple distillation and obtain triisopropyl borate ester;
E: in rectifying tower the water of telling among the step b is carried out the sequence of constant boiling and rectification at intermittence, the Virahol of recovery and nonvariant boiling reagent join among the step b.
2. the production method of a kind of high-purity triisopropyl borate ester according to claim 1, it is characterized in that: the boric acid that adds among the described step a and the ratio of Virahol are 1: 3.5～6.
3. the production method of a kind of high-purity triisopropyl borate ester according to claim 1, it is characterized in that: the ratio of described step b mesoboric acid and nonvariant boiling reagent is 1: 1.5～2.6.
4. the production method of a kind of high-purity triisopropyl borate ester according to claim 1, it is characterized in that: the temperature of reactive distillation is 82 ℃～86 ℃ among the described step b.
5. the production method of a kind of high-purity triisopropyl borate ester according to claim 1 is characterized in that: among the described step b in the nonvariant boiling reagent ratio of each component be benzene: toluene: hexanaphthene equals 3: 1: 1.
6. the production method of a kind of high-purity triisopropyl borate ester according to claim 1, it is characterized in that: the batch fractionating of described step c or step e intermittence sequence of constant boiling and rectification for carrying out the binary batch fractionating earlier, divide dried up and nonvariant boiling reagent, carry out ternary sequence of constant boiling and rectification at intermittence again and isolate Virahol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2007101797162A CN101463041B (en) | 2007-12-17 | 2007-12-17 | Production method of high-purity triisopropyl borate ester |
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| CN2007101797162A CN101463041B (en) | 2007-12-17 | 2007-12-17 | Production method of high-purity triisopropyl borate ester |
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| CN101463041A CN101463041A (en) | 2009-06-24 |
| CN101463041B true CN101463041B (en) | 2011-08-31 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104356152A (en) * | 2014-11-07 | 2015-02-18 | 白银摩尔化工有限责任公司 | Method for producing high-purity triisopropyl borate through system external circulation reaction dehydration |
| WO2018042925A1 (en) * | 2016-09-05 | 2018-03-08 | 日立化成株式会社 | Additive for electrochemical elements, electrolyte solution for electrochemical elements, electrochemical element, electrolyte solution for lithium ion secondary batteries, lithium ion secondary battery and method for producing additive for electrochemical elements |
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Non-Patent Citations (2)
| Title |
|---|
| 徐前永等.硼酸三异丙酯合成方法的改进.《化学试剂》.2004,第26卷(第4期), * |
| 陈宏刚等.硼酸酯类偶联剂的合成.《塑料科技》.1996,(第2期), * |
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Inventor after: Li Xiaobao Inventor after: Qian Bingrong Inventor before: Qian Bingrong Inventor before: Li Xiaobao |
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Free format text: CORRECT: INVENTOR; FROM: QIAN BINGRONG LI XIAOBAO TO: LI XIAOBAO QIAN BINGRONG |
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Effective date of registration: 20180809 Address after: 226500 Jiangsu, Nantong, Rugao, Changjiang town (Rugao port) Fine Chemical Industrial Park Pujiang Road No. 1 Patentee after: Jiangsu Acer Zixin Energy Technology Co Ltd Address before: 226500 1 Gaoyang West Road, Linzi Town, Rugao, Jiangsu Patentee before: Nantong Hongzhi Chemical Co., Ltd. |