CN114516887A - Preparation method of triisopropyl borate - Google Patents
Preparation method of triisopropyl borate Download PDFInfo
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- CN114516887A CN114516887A CN202210076670.6A CN202210076670A CN114516887A CN 114516887 A CN114516887 A CN 114516887A CN 202210076670 A CN202210076670 A CN 202210076670A CN 114516887 A CN114516887 A CN 114516887A
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- rectification
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- isopropanol
- borate
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- NHDIQVFFNDKAQU-UHFFFAOYSA-N tripropan-2-yl borate Chemical compound CC(C)OB(OC(C)C)OC(C)C NHDIQVFFNDKAQU-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 86
- 238000006243 chemical reaction Methods 0.000 claims abstract description 43
- WRECIMRULFAWHA-UHFFFAOYSA-N trimethyl borate Chemical compound COB(OC)OC WRECIMRULFAWHA-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000004519 manufacturing process Methods 0.000 claims abstract description 28
- 239000002253 acid Substances 0.000 claims abstract description 16
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 14
- 239000003054 catalyst Substances 0.000 claims description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- 238000007171 acid catalysis Methods 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 229940098779 methanesulfonic acid Drugs 0.000 claims description 3
- WBHQBSYUUJJSRZ-UHFFFAOYSA-M sodium bisulfate Chemical compound [Na+].OS([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-M 0.000 claims description 3
- 229910000342 sodium bisulfate Inorganic materials 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- 238000005809 transesterification reaction Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 9
- 238000011112 process operation Methods 0.000 abstract description 6
- 238000000926 separation method Methods 0.000 abstract description 6
- 125000004185 ester group Chemical group 0.000 abstract description 5
- 238000009776 industrial production Methods 0.000 abstract description 5
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 239000007858 starting material Substances 0.000 abstract description 3
- 238000004904 shortening Methods 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 239000000047 product Substances 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 9
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 5
- 239000004327 boric acid Substances 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 5
- -1 oxonium ion Chemical class 0.000 description 5
- 238000009835 boiling Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 3
- 238000000998 batch distillation Methods 0.000 description 3
- 229910052796 boron Inorganic materials 0.000 description 3
- 239000012043 crude product Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000002360 explosive Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- CSDQQAQKBAQLLE-UHFFFAOYSA-N 4-(4-chlorophenyl)-4,5,6,7-tetrahydrothieno[3,2-c]pyridine Chemical compound C1=CC(Cl)=CC=C1C1C(C=CS2)=C2CCN1 CSDQQAQKBAQLLE-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000012024 dehydrating agents Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000000066 reactive distillation Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 238000010626 work up procedure Methods 0.000 description 2
- 238000010533 azeotropic distillation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- JYVHOGDBFNJNMR-UHFFFAOYSA-N hexane;hydrate Chemical compound O.CCCCCC JYVHOGDBFNJNMR-UHFFFAOYSA-N 0.000 description 1
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 125000003253 isopropoxy group Chemical group [H]C([H])([H])C([H])(O*)C([H])([H])[H] 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000000269 nucleophilic effect Effects 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 238000011027 product recovery Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000013341 scale-up Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000009270 solid waste treatment Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for preparing triisopropyl borate, which comprises the steps of taking trimethyl borate as a starting material, carrying out ester exchange reaction with isopropanol under the catalysis of acid, and carrying out post-treatment by simple rectification separation to obtain the triisopropyl borate with high purity and high yield. The method has mild reaction conditions, simple system after the reaction is finished and few components, and only simple rectification equipment is used for continuous rectification once, thereby greatly reducing the requirements on the equipment, simplifying the process operation, improving the production safety, greatly shortening the production period, improving the production efficiency and being particularly suitable for large-scale industrial production.
Description
Technical Field
The invention relates to a preparation method of triisopropyl borate, belonging to the technical field of organic synthesis.
Background
The triisopropyl borate is colorless transparent liquid, is mainly used as a solvent and a semiconductor boron diffusion source, and is an important organic boron fine chemical raw material.
The existing production method of triisopropyl borate comprises the steps of reacting boric anhydride or boric acid serving as a starting material with isopropanol, and then obtaining the high-purity triisopropyl borate through more complex binary batch rectification and ternary batch rectification. For example, a paper "improvement of a method for synthesizing triisopropyl borate" published in "chemical reagent" discloses a method for synthesizing triisopropyl borate from boric anhydride and isopropyl alcohol as raw materials by using calcium hydride as a dehydrating agent.
Chinese patent CN201210009269.7 discloses a method for producing high-purity triisopropyl borate, which comprises the steps of adding reactants of boric anhydride, water, isopropanol and cyclohexane into a tower kettle, using the cyclohexane as an azeotropic agent, reacting the boric anhydride and the water under the conditions of 0.1 MPa of pressure and 80-100 ℃ to generate boric acid, carrying out reactive distillation on the boric acid, the isopropanol and the cyclohexane to obtain a crude product containing the triisopropyl borate, continuously carrying out binary batch distillation and ternary batch distillation on the triisopropyl borate crude product in the tower kettle, respectively separating the cyclohexane and the isopropanol, refluxing from the tower top, separating water, separating a mixture of the cyclohexane and the isopropanol in a separation tank to a mixture recovery box, re-entering the tower kettle to carry out the distillation reaction, separating the triisopropyl borate to a finished product recovery box, and collecting a finished product.
Chinese patent CN200710179716.2 also discloses a method for producing high-purity triisopropyl borate, which comprises the steps of taking boric acid and isopropanol as raw materials, taking a mixture of benzene, toluene and cyclohexane as an azeotropic agent, carrying out reactive distillation in a kettle-type reactor, separating water and the azeotropic agent through binary batch distillation, and then carrying out ternary batch azeotropic distillation to separate the isopropanol. The patent adopts a reaction rectification technology of adding an azeotropic agent to separate by-product water from a reaction system, improves the conversion rate of the reaction, and solves the defects of inconvenient operation, difficult solid waste treatment and high operation risk of a calcium hydride dehydrating agent; meanwhile, the crude product is refined by adopting a novel batch rectification technology with a tower top storage tank, so that the high-purity triisopropyl borate can be obtained, and the recovered isopropanol and the azeotropic agent can be recycled.
As can be seen from the prior art, the existing preparation of triisopropyl borate takes boric anhydride or boric acid as an initial raw material, and after the reaction with isopropanol is completed, the triisopropyl borate with high purity can be obtained only by relatively complex binary batch rectification and ternary batch rectification, so the required device and equipment are complex, and the process operation is complicated; and in the subsequent separation process, flammable and explosive dangerous chemicals such as benzene and cyclohexane are involved, so that the production process is poor in safety. Because the operation is complicated, the production period in the prior art is long, and one period can be completed generally within 24-48 hours. In addition, water is generated in the reaction process, if the water is not removed in time or is not completely removed, the reaction is not complete, mono-substituted products and di-substituted products are easy to appear, and the purity of the product is influenced.
How to solve the problems in the prior art, simplify the production process of triisopropyl borate, reduce the requirements on equipment, shorten the production period and improve the safety is a technical problem to be solved urgently by technical personnel in the field.
Disclosure of Invention
The invention aims to provide a method for preparing triisopropyl borate, which comprises the steps of taking trimethyl borate as a starting material, carrying out ester exchange reaction with isopropanol under the catalysis of acid, and carrying out post-treatment by simple rectification separation to obtain the triisopropyl borate with high purity and high yield. The method has mild reaction conditions, greatly reduces the requirements on equipment, simplifies the process operation, improves the production safety, greatly shortens the production period, and has great advantages in large-scale industrial production.
The invention provides a preparation method of triisopropyl borate, which is characterized in that trimethyl borate shown in a formula (I) and isopropanol are subjected to transesterification reaction under the acid catalysis condition to obtain triisopropyl borate shown in a formula (II)
According to a particular but non-limiting embodiment of the invention, the preparation process comprises: under the protection of inert gas, adding isopropanol and catalyst acid into a reaction container, controlling the temperature at 30-70 ℃, slowly adding trimethyl borate shown in the formula (I), preserving the temperature at 30-70 ℃ for 3-4 hours, and after the reaction is finished, separating and purifying through common rectification to obtain triisopropyl borate shown in the formula (II).
According to a particular but non-limiting embodiment of the invention, wherein the rectification is carried out at a controlled temperature of 20 to 60 ℃ and a pressure of-0.1 to-0.07 mpa, triisopropyl borate is obtained by rectification.
According to a particular but non-limiting embodiment of the invention, wherein the work-up employs a single continuous rectification.
According to a particular but non-limiting embodiment of the invention, wherein the rectification is carried out using a common rectification column.
According to a particular but non-limiting embodiment of the invention, wherein the excess isopropanol is recovered by rectification, it is not necessary to work up directly for the next reaction.
According to a particular but non-limiting embodiment of the invention, wherein the molar ratio of isopropanol to trimethyl borate is between 3 and 5: 1.
according to a specific but non-limiting embodiment of the invention, wherein the catalyst acid is selected from at least one of p-toluenesulfonic acid, methanesulfonic acid, concentrated sulfuric acid, sodium bisulfate, phosphoric acid and concentrated hydrochloric acid.
According to a particular but non-limiting embodiment of the invention, wherein the molar ratio of the catalyst acid to trimethyl borate is between 0.02 and 1: 1.
according to a specific but non-limiting embodiment of the invention, wherein the molar ratio of isopropanol to trimethyl borate is 4.3: 1; the molar ratio of the catalyst acid to trimethyl borate is 0.03: 1.
the invention has the following beneficial effects:
1. the invention uses trimethyl borate to prepare triisopropyl borate through ester exchange reaction with isopropanol under the catalysis of acid, the system after the reaction is finished is simple, the components are few, the product with high purity and high yield can be obtained through one-time continuous rectification by using simple rectification equipment, the process operation is greatly simplified, the requirement on the equipment is reduced, and the invention is particularly suitable for large-scale industrial production.
2. In the post-treatment separation process, except the product, only the generated methanol and the residual trace isopropanol are generated, and flammable and explosive dangerous goods are not involved, so that the safety degree is high.
3. The method is simple, only 16-20 hours are needed for one production cycle, and compared with the prior art that one cycle is 24-48 hours, the time is greatly shortened, and the production efficiency is improved.
4. The invention avoids the problems of water generation and water removal through ester exchange reaction, and is easy to obtain high-purity products.
Drawings
FIG. 1 is a nuclear magnetic spectrum of triisopropyl borate prepared in example 1 of the present invention.
Detailed Description
The following specific embodiments are provided to further illustrate the present invention, but the present invention is not limited to only the following embodiments.
The invention provides a preparation method of triisopropyl borate, which is suitable for industrial production and comprises the following steps: under the condition of acid catalysis, trimethyl borate shown in the formula (I) and isopropanol are subjected to transesterification reaction to obtain triisopropyl borate shown in the formula (II). The reaction formula of the invention is as follows:
the reaction mechanism of the present invention is as follows:
an oxygen atom on trimethyl borate is firstly combined with a hydrogen ion to form an oxonium ion, then isopropanol carries out nucleophilic attack on a boron atom, and simultaneously, a methanol molecule is lost, so that the substitution reaction of an isopropyloxy group on a methoxyl group is completed. In the same way, the other two methoxyl groups are substituted by the isopropoxy group, and the triisopropyl borate is finally obtained.
The system after the reaction is finished is simple, and the components are triisopropyl borate (boiling point 139 ℃), the generated methanol (boiling point 65.4 ℃) and the residual isopropanol (boiling point 82 ℃). Because the boiling points of the three components have larger difference, the three components can be separated by simple rectification, thereby greatly reducing the requirements on equipment and simplifying the original complicated process operation.
Specifically, the preparation method comprises the following steps: under the protection of inert gas, adding isopropanol and catalyst acid into a reaction container, controlling the temperature at 30-70 ℃, slowly adding trimethyl borate shown in the formula (I), preserving the temperature at 30-70 ℃ for 3-4 hours, and after the reaction is finished, separating and purifying through common rectification to obtain triisopropyl borate shown in the formula (II).
Wherein the rectification is carried out under the conditions that the temperature is controlled to be 20-60 ℃ and the pressure is-0.1 to-0.07 mpa, and triisopropyl borate is obtained by rectification.
Isopropanol is both a reactant and a solvent. The molar ratio of isopropanol to trimethyl borate is usually 3-5: 1; preferably 4.3: 1.
the catalyst acid may be at least one selected from the group consisting of p-toluenesulfonic acid, methanesulfonic acid, concentrated sulfuric acid, sodium bisulfate, phosphoric acid, concentrated hydrochloric acid, and the like, and p-toluenesulfonic acid is preferably used. The molar ratio of the catalyst acid to the trimethyl borate is usually 0.02-1: 1; preferably 0.03: 1. the catalyst acid has important influence on the reaction, so that the reaction can smoothly complete trisubstitution, and the obtained main product is a trisubstituent instead of a mono-substituent and a di-substituent.
It was found by experiment that when the molar ratio of the catalyst acid to trimethyl borate reached 0.03: 1, the molar ratio of isopropanol to trimethyl borate is 4.3: at 1, the conversion of the reaction just reached 100%.
Because the system after the reaction is simple and the components are few, the post-treatment can be separated by one-time continuous rectification to obtain the high-purity triisopropyl borate without multiple rectification, and the excessive isopropanol can be recycled by rectification and can be directly applied to the next reaction without treatment. In large-scale industrial production, the invention can finish the separation and purification of products by using a common rectifying tower, has very simple requirements on equipment and devices, and has very simple and convenient process operation.
Except for the product of triisopropyl borate, the system after the reaction only contains the generated methanol and trace unreacted isopropanol, does not relate to benzene, toluene, cyclohexane and other flammable and explosive dangerous goods, and has good production process safety.
According to the invention, trimethyl borate and isopropanol are used for preparing triisopropyl borate through ester exchange reaction, water is not generated in the reaction process, the problems of water removal and generation of impurities such as mono-substituent, di-substituent and the like are avoided, and the obtained product has high purity and high yield. Experiments prove that the yield of the triisopropyl borate prepared by the method is up to more than 90 percent, and the purity of the triisopropyl borate prepared by the method can be up to more than 99.5 percent. Generally, one production cycle of the invention only needs 16-20 hours, while one production cycle of the prior art needs 24-48 hours, the invention obviously shortens the production time and improves the production efficiency.
The present invention will be further illustrated with reference to the following specific examples, but the present invention is not limited to the following examples.
The experimental procedures used above and in the examples below are conventional unless otherwise specified.
The materials, reagents and the like used above and in the following examples are commercially available unless otherwise specified.
Example 1
Under the protection of nitrogen, 500g of isopropanol and 10g of p-toluenesulfonic acid are added into a 1L four-mouth bottle, the temperature is raised to 55 ℃, and 200g of trimethyl borate is slowly added. After the addition, the temperature is kept at 50 ℃ for 3.5h, the sample is taken and sent to the gas phase, the trimethyl borate is completely converted to triisopropyl borate, and the reaction is finished. Controlling the temperature to be 40-50 ℃, and the pressure to be-0.1-0.07 mpa, obtaining 333.0g of triisopropyl borate through ordinary rectification, wherein the yield is 92%, and the GC purity is 99.5%. And rectifying to recover isopropanol, and directly sleeving the recovered isopropanol for the next reaction. FIG. 1 is a nuclear magnetic spectrum of triisopropyl borate prepared in example 1.
Example 2
600g of isopropanol (part of the isopropanol recovered in example 1) and 10g of p-toluenesulfonic acid were added to a 1L four-necked flask under nitrogen protection, and 200g of trimethyl borate was slowly added thereto while raising the temperature to 60 ℃. After the addition, the temperature is kept at 60 ℃ for 3.5h, the sample is taken and sent to the gas phase, the trimethyl borate is completely converted to triisopropyl borate, and the reaction is finished. The temperature is controlled to be 40-50 ℃, the pressure is controlled to be-0.1-0.07 mpa, 334.1g of triisopropyl borate is obtained by ordinary rectification, the yield is 92.3 percent, and the GC purity is 99.6 percent. And rectifying to recover isopropanol, and directly sleeving the recovered isopropanol for the next reaction.
Example 3
Industrial scale-up preparation example
Under the protection of nitrogen, 500Kg of isopropanol and 10Kg of p-toluenesulfonic acid are added into a 1000L reaction kettle, the temperature is raised to 55 ℃, and 200Kg of trimethyl borate is slowly added. After the addition, the temperature is kept at 50 ℃ for 3.5h, the sample is taken and sent to the gas phase, the trimethyl borate is completely converted to triisopropyl borate, and the reaction is finished. The triisopropyl borate is rectified to obtain 336.0Kg by a rectifying tower with the height of 5 m, the temperature is controlled to be 40-50 ℃, and the pressure is-0.1 to-0.07 mpa, the yield is 92.8 percent, and the GC purity is 99.6 percent. And rectifying to recover isopropanol, and directly sleeving the recovered isopropanol for the next reaction.
The above is only a specific application example of the present invention, and the protection scope of the present invention is not limited in any way. All the technical solutions formed by equivalent transformation or equivalent replacement fall within the protection scope of the present invention.
Claims (10)
1. The preparation method of triisopropyl borate is characterized in that trimethyl borate shown in formula (I) and isopropanol are subjected to transesterification reaction under the acid catalysis condition to obtain triisopropyl borate shown in formula (II)
2. The production method according to claim 1, comprising: under the protection of inert gas, adding isopropanol and catalyst acid into a reaction container, controlling the temperature at 30-70 ℃, slowly adding trimethyl borate shown in the formula (I), preserving heat at 30-70 ℃ for 3-4 hours, and after the reaction is finished, separating and purifying through common rectification to obtain triisopropyl borate shown in the formula (II).
3. The production process according to claim 2, wherein the rectification is carried out at a temperature of 20 to 60 ℃ and a pressure of-0.1 to-0.07 mpa to obtain triisopropyl borate by rectification.
4. The production process according to any one of claims 1 to 3, wherein the post-treatment employs a single continuous rectification.
5. The production method according to any one of claims 1 to 3, wherein the rectification is performed using one common rectification column.
6. The production process according to any one of claims 1 to 3, wherein the excess isopropyl alcohol is recovered by rectification without being disposed of directly for the next reaction.
7. The production method according to any one of claims 1 to 3, wherein the molar ratio of isopropanol to trimethyl borate is 3 to 5: 1.
8. the production method according to any one of claims 1 to 3, wherein the catalyst acid is at least one selected from the group consisting of p-toluenesulfonic acid, methanesulfonic acid, concentrated sulfuric acid, sodium hydrogensulfate, phosphoric acid and concentrated hydrochloric acid.
9. The production method according to any one of claims 1 to 3, wherein the molar ratio of the catalyst acid to trimethyl borate is 0.02 to 1: 1.
10. the production method according to claim 3, wherein the molar ratio of isopropanol to trimethyl borate is 4.3: 1; the molar ratio of the catalyst acid to trimethyl borate is 0.03: 1.
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| CN103204866A (en) * | 2012-01-12 | 2013-07-17 | 金良玉 | Production method of high purity triisopropyl borate |
| 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 |
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2022
- 2022-01-24 CN CN202210076670.6A patent/CN114516887A/en active Pending
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|---|---|---|---|---|
| FR1225080A (en) * | 1958-02-21 | 1960-06-29 | United States Borax Chem | Process for preparing alkyl borate esters |
| GB842534A (en) * | 1958-02-21 | 1960-07-27 | United States Borax Chem | Method of preparing alkyl borate esters |
| FR1284235A (en) * | 1961-03-14 | 1962-02-09 | Exxon Research Engineering Co | Manufacturing process of higher boron compounds and derived alcohols |
| JP2013010913A (en) * | 2011-05-27 | 2013-01-17 | Sanko Kagaku Kogyo Kk | Antistatic composition, and molded object, coating material, antistatic coated object and pressure-sensitive adhesive using the same, and method for producing the same |
| CN103204866A (en) * | 2012-01-12 | 2013-07-17 | 金良玉 | Production method of high purity triisopropyl borate |
| 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 |
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