CN116041379B - Environment-friendly manufacturing method and matched manufacturing equipment for electronic grade trimethyl borate - Google Patents
Environment-friendly manufacturing method and matched manufacturing equipment for electronic grade trimethyl borate Download PDFInfo
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- CN116041379B CN116041379B CN202310166079.4A CN202310166079A CN116041379B CN 116041379 B CN116041379 B CN 116041379B CN 202310166079 A CN202310166079 A CN 202310166079A CN 116041379 B CN116041379 B CN 116041379B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
- B01D3/146—Multiple effect distillation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0492—Applications, solvents used
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- 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 System
- C07F5/02—Boron compounds
- C07F5/04—Esters of boric acids
Abstract
The invention discloses an environment-friendly manufacturing method of electronic grade trimethyl borate and matched preparation equipment, wherein the environment-friendly preparation equipment is provided with a raw material treatment assembly, a crude distillation kettle assembly, a pre-extraction assembly and a triple nitrogen protection distillation kettle assembly in the order from feeding to discharging; wherein a solid-liquid separation device and a crude fraction detection device are arranged between the crude distillation kettle component and the pre-extraction component; a nitrogen protection extractant evaporating device and a prefabricated fraction detecting device are sequentially arranged between the pre-extraction component and the triple nitrogen protection rectifying still component; the pre-extraction component is also provided with an upper layer extraction and delivery device which is matched with the feed inlet of the crude distillation kettle component; the crude distillation kettle component and the triple nitrogen protection distillation kettle component are both provided with a condensing device and a reflux control device. The invention has the advantages of environment-friendly production process, simple raw material types, low cost, stable and controllable process and high product purity.
Description
Technical Field
The invention relates to a manufacturing device and a using method of electronic grade trimethyl borate, in particular to an environment-friendly manufacturing method and matched preparation equipment of electronic grade trimethyl borate.
Background
Trimethyl borate (TMB), molecular formula: (CH) 3 O 3 ) B, mainly used for depositing and generating borophosphosilicate glass (BPSG) in the wafer manufacturing process, is an important electronic chemical required by semiconductor, discrete device and micro-electromechanical system (MEMS) manufacturing. Trimethyl borate was used early as an organic solvent, plasticizer, catalyst, welding flux and flame retardant. Sulfuric acid is commonly used in industry as a catalyst to catalyze the synthesis of trimethyl borate from boric acid and methanol. Sulfuric acid is used as a catalyst, and has the disadvantages of low price, high activity, more byproducts, difficult separation, high corrosion to equipment and the like.
TMB and methanol form a binary homogeneous constant boiling point of 54.6 ℃ and the mass percent of methanol in the homogeneous constant boiling point is 25%. Carbon disulfide and methanol form binary heterogeneous constant boiling substances, the boiling point is 38 ℃, and the mass percentage of the methanol is 14%. Adding carbon disulfide into TMB-methanol azeotropic mixture for rectification, distilling carbon disulfide-methanol azeotropic mixture at the top of the tower, and then flowing out the carbon disulfide to finally obtain TMB. The carbon disulfide-methanol azeotropic mixture is heterogeneous azeotropic mixture, two liquid phases are formed after standing, and the lower carbon disulfide layer (containing 97% of carbon disulfide and 3% of methanol) flows back into the rectifying tower. If the carbon disulfide-methanol azeotrope contains a small amount of TMB (1.5%), it is difficult for the azeotrope to form a heterogeneous phase. Therefore, the separation degree of the rectification process is highly demanded. In addition to carbon disulphide, pentane, methylpentane, dimethylpentane, and chloropentane may be used. Because the boiling point of the new constant boiling point material is low, the additional solvent needs to be recovered after vaporization and condensation, the energy consumption is high, the investment is large, and the method is not suitable for industrial production.
Therefore, an environment-friendly manufacturing method and matched preparation equipment for electronic grade trimethyl borate with environment-friendly production process, simple raw material types, low cost, stable and controllable process and high product purity are needed at present.
Disclosure of Invention
The invention aims to provide an environment-friendly manufacturing method and matched preparation equipment of electronic grade trimethyl borate, which have the advantages of environment-friendly production process, simple raw material types, low cost, stable and controllable process and high product purity.
In order to achieve the above purpose, the present invention adopts the following technical scheme: a process for preparing electronic grade trimethyl borate, comprising the following stages:
s1: raw material preparation
(1) Raw material preparation: preparing sufficient boric acid and methanol;
(2) preparing auxiliary materials: preparing a sufficient amount of tri-2-decyl tetradecanoate glyceride and a sufficient amount of lithium chloride;
s2: pure manufacture of crude trimethyl borate
(1) Weighing 9.8-10.2 parts by weight of boric acid, drying the boric acid at 145-150 ℃ for 6-8 hours, and mechanically grinding the boric acid to a particle size not greater than 0.1mm to obtain dried boric acid powder, wherein the step is completed in a raw material treatment assembly;
(2) uniformly mixing the dried boric acid powder obtained in the step (1) with 18-18.5 parts of methanol solution by weight, putting into a crude distillation kettle assembly, setting heating reflux time to be 4-4.5 hours, then collecting a front fraction in a temperature section of 54-55 ℃, and collecting a rear fraction in a temperature section of 56-70 ℃; wherein the rear fraction is used for recovering and extracting methanol; the front-end fraction is sent to a pre-extraction component;
s3: pre-purification
(1) Adding a sufficient amount of the tri-2-decyl tetradecanoate glyceride and lithium chloride prepared in the step (2) of the step S1 into the front cut of the step (2) of the step S2 injected into the pre-extraction assembly 4; the specific standard of the sufficient amount is that lithium chloride and alcohol in the front fraction form saturated solution, tri-2-decyl tetradecanoate glyceride can completely dissolve trimethyl borate in the front fraction, the mixture is stirred and then is stood for layering, the upper layer is an alcohol layer, the lower layer is an ester layer, and the lower layer of ester layer solution is sent to a nitrogen protection extractant steaming device; distilling the upper alcohol layer solution to separate lithium chloride, and then partially refluxing and injecting the alcohol solution into a feed inlet of the crude distillation kettle component;
(3) filling sufficient nitrogen into a nitrogen protection extractant evaporation device to discharge air, setting heating reflux time to be 3.5-4 h, and collecting a fraction at a temperature of 68-70 ℃ to obtain prepurified trimethyl borate;
(4) sending the prepurified trimethyl borate obtained in the step (3) into a prefabricated fraction detection device, and sending the qualified prepurified trimethyl borate into a triple nitrogen protection rectifying kettle component for rectification if the purity of the trimethyl borate is required to be not lower than 99.9%;
s4: rectifying
(1) Putting the qualified prepurified trimethyl borate obtained in the step S3 and the step (4) into a 1-stage rectifying tower in a triple nitrogen protection rectifying still assembly, heating by an oil bath partition wall, enabling gas phase to escape to a tower plate, opening a rectifying product collecting valve and a storage tank valve after a plurality of condensation and vaporization processes, introducing trimethyl borate into the 1-stage rectifying product storage tank, and opening a 1-stage rectifying product storage tank discharging valve and a rectifying tower continuous feeding regulating valve for continuous feeding production;
(2) putting the grade 1 rectification product into a grade 2 rectification tower, repeating the step (1), introducing trimethyl borate into a grade 2 rectification product storage tank, opening a discharging valve of the grade 2 rectification product storage tank and a continuous feeding regulating valve of the rectification tower, and continuously feeding for production;
(3) putting the 2-level rectification product into a 3-level rectification tower, repeating the step (1), and introducing trimethyl borate into a 2-level rectification product storage tank to obtain the required electronic-level trimethyl borate;
s5: detection of
(1) Detecting the electronic grade trimethyl borate obtained in the step (3) in the step S4, wherein the purity of the main fraction trimethyl borate is required to be not lower than 99.99 percent, and entering a trace impurity detection program if the purity is qualified;
(2) detecting trace impurities in the electronic grade trimethyl borate in the step S4, wherein the total content of the impurities is required to be not higher than 0.0000005% (8.5N), and entering a packaging program if the total content of the impurities is qualified;
the environment-friendly preparation equipment matched with the process method is provided with a raw material treatment assembly, a crude distillation kettle assembly, a pre-extraction assembly and a triple nitrogen protection distillation kettle assembly in the sequence from feeding to discharging; wherein a solid-liquid separation device and a crude fraction detection device are arranged between the crude distillation kettle component and the pre-extraction component; a nitrogen protection extractant evaporating device and a prefabricated fraction detecting device are sequentially arranged between the pre-extraction component and the triple nitrogen protection rectifying still component; the pre-extraction component is also provided with an upper layer extraction and delivery device which is matched with the feed inlet of the crude distillation kettle component; the crude distillation kettle component and the triple nitrogen protection distillation kettle component are both provided with a condensing device and a reflux control device;
compared with the prior art, the invention has the following advantages due to the adoption of the technical scheme:
(1) The invention does not adopt any harmful catalytic substances such as concentrated sulfuric acid and the like, and the whole process is environment-friendly.
(2) Besides the main raw material components, all the extraction auxiliary materials and the additive components can be completely recovered, and the method is circulated and used without increasing the extraction cost, so that the method has the advantages of simple components, low cost and suitability for industrial production.
(3) Compared with the conventional technology, the method has the advantages that the synthetic route is longer, the production period is longer, but the different purification technologies are adopted, the complementary impurity removal is realized, the quality of the final product is more controllable, the index is 99.99% of the purity of the main fraction, the trace impurity content of 8.5N level can practically reach more than 99.997% of the purity of the main fraction, and the trace impurity content of 9N level is higher than the purity of commercial electronic grade trimethyl borate.
Therefore, the invention has the characteristics of environmental protection in the production process, simple raw material types, low cost, stable and controllable process and high product purity.
Drawings
FIG. 1 is a schematic diagram of the structure of the present invention;
FIG. 2 is a graph showing quality metrics of the present invention;
in the figure: the device comprises a crude distillation kettle component 1, a solid-liquid separation device 2, a crude fraction detection device 3, a pre-extraction component 4, a condensation device 5, a reflux control device 6, a triple nitrogen protection distillation kettle component 7, a nitrogen protection extractant distillation device 8 and a prefabricated fraction detection device 9.
Description of the embodiments
Examples
A process for preparing electronic grade trimethyl borate, comprising the following stages:
s1: raw material preparation
(1) Raw material preparation: preparing sufficient boric acid and methanol;
(2) preparing auxiliary materials: preparing a sufficient amount of tri-2-decyl tetradecanoate glyceride and a sufficient amount of lithium chloride;
s2: pure manufacture of crude trimethyl borate
(1) Weighing 9.8-10.2 parts by weight of boric acid, drying the boric acid at 145-150 ℃ for 6-8 hours, and mechanically grinding the boric acid to a particle size not greater than 0.1mm to obtain dried boric acid powder, wherein the step is completed in a raw material treatment assembly;
(2) uniformly mixing the dried boric acid powder obtained in the step (1) with 18-18.5 parts of methanol solution by weight, putting the mixture into a crude distillation kettle assembly 1, setting heating reflux time to be 4-4.5 hours, then collecting a front fraction in a temperature section of 54-55 ℃, and collecting a rear fraction in a temperature section of 56-70 ℃; wherein the rear fraction is used for recovering and extracting methanol; the front-end fraction is sent to a pre-extraction assembly 4;
s3: pre-purification
(1) Adding a sufficient amount of the tri-2-decyl tetradecanoate glyceride and lithium chloride prepared in the step (2) of the step S1 into the front cut of the step (2) of the step S2 injected into the pre-extraction assembly 4; the specific standard of the sufficient amount is that lithium chloride and alcohol in the front fraction form saturated solution, tri-2-decyl tetradecanoate glyceride can completely dissolve trimethyl borate in the front fraction, the mixture is stirred and then is stood for layering, the upper layer is an alcohol layer, the lower layer is an ester layer, and the lower layer of ester layer solution is sent to a nitrogen protection extractant steaming device 8; distilling the upper alcohol layer solution to separate lithium chloride, and then partially refluxing and injecting the alcohol solution into a feed inlet of the crude distillation kettle assembly 1;
(3) filling sufficient nitrogen into the nitrogen protection extractant evaporation device 8 to discharge air, setting heating reflux time to be 3.5-4 h, and collecting a fraction at a temperature of 68-70 ℃ to obtain prepurified trimethyl borate;
(4) sending the prepurified trimethyl borate obtained in the step (3) to a prefabricated fraction detection device 9, and sending the qualified prepurified trimethyl borate to a triple nitrogen protection rectifying kettle component 7 for rectification if the purity of the trimethyl borate is required to be not lower than 99.9%;
s4: rectifying
(1) Putting qualified prepurified trimethyl borate obtained in the step S3 and the step (4) into a 1-stage rectifying tower in a triple nitrogen protection rectifying still assembly 7, heating by an oil bath partition wall, enabling gas phase to escape to a tower plate, opening a rectification product collecting valve and a storage tank valve after a plurality of condensation and vaporization processes, introducing trimethyl borate into the 1-stage rectification product storage tank, opening a 1-stage rectification product storage tank discharging valve and a rectifying tower continuous feeding regulating valve, and continuously feeding for production;
(2) putting the grade 1 rectification product into a grade 2 rectification tower, repeating the step (1), introducing trimethyl borate into a grade 2 rectification product storage tank, opening a discharging valve of the grade 2 rectification product storage tank and a continuous feeding regulating valve of the rectification tower, and continuously feeding for production;
(3) putting the 2-level rectification product into a 3-level rectification tower, repeating the step (1), and introducing trimethyl borate into a 2-level rectification product storage tank to obtain the required electronic-level trimethyl borate;
s5: detection of
(1) Detecting the electronic grade trimethyl borate obtained in the step (3) in the step S4, wherein the purity of the main fraction trimethyl borate is required to be not lower than 99.995%, and entering a trace impurity detection program if the purity is qualified;
(2) detecting trace impurities in the electronic grade trimethyl borate in the step S4, wherein the total content of the impurities is required to be not higher than 0.0000005% (8.5N), and entering a packaging program if the total content of the impurities is qualified;
the environment-friendly preparation equipment of the electronic grade trimethyl borate shown in the figure 1 is matched with the process method, and is provided with a raw material treatment assembly, a crude distillation kettle assembly 1, a pre-extraction assembly 4 and a triple nitrogen protection distillation kettle assembly 7 in the sequence from feeding to discharging; wherein a solid-liquid separation device 2 and a crude fraction detection device 3 are arranged between the crude distillation kettle assembly 1 and the pre-extraction assembly 4; a nitrogen protection extractant evaporation device 8 and a prefabricated fraction detection device 9 are sequentially arranged between the pre-extraction component 4 and the triple nitrogen protection rectifying still component 7; the pre-extraction component is also provided with an upper layer extraction and delivery device which is matched with the feed inlet of the crude distillation kettle component 1; the crude distillation kettle component 1 and the triple nitrogen protection distillation kettle component 7 are respectively provided with a condensing device 5 and a reflux control device 6.
As shown in FIG. 2, the electron-grade trimethyl borate (TMB) produced according to the method of this example had a purity of not less than 99.99% and a total impurity content of not more than 0.0000005%.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (1)
1. The process method for preparing the electronic grade trimethyl borate is characterized by comprising the following steps of:
s1: raw material preparation
(1) Raw material preparation: preparing sufficient boric acid and methanol;
(2) preparing auxiliary materials: preparing a sufficient amount of tri-2-decyl tetradecanoate glyceride and a sufficient amount of lithium chloride;
s2: pure manufacture of crude trimethyl borate
(1) Weighing 9.8-10.2 parts by weight of boric acid, drying the boric acid at 145-150 ℃ for 6-8 hours, and mechanically grinding the boric acid to a particle size not greater than 0.1mm to obtain dried boric acid powder, wherein the step is completed in a raw material treatment assembly;
(2) uniformly mixing the dried boric acid powder obtained in the step (1) with 18-18.5 parts of methanol solution by weight, putting the mixture into a crude distillation kettle assembly (1), setting heating reflux time to be 4-4.5 hours, then collecting a front fraction in a temperature section of 54-55 ℃, and collecting a rear fraction in a temperature section of 56-70 ℃; wherein the rear fraction is used for recovering and extracting methanol; the front-end fraction is sent to a pre-extraction assembly (4);
s3: pre-purification
(1) Adding a sufficient amount of the tri-2-decyl tetradecanoate glyceride and lithium chloride prepared in the step (2) of the step S1 into the front cut of the step (2) of the step S2 injected into the pre-extraction component (4); the specific standard of the sufficient amount is that lithium chloride and alcohol in the front fraction form saturated solution, tri-2-decyl tetradecanoate glyceride can completely dissolve trimethyl borate in the front fraction, the mixture is stirred and then is stood for layering, the upper layer is an alcohol layer, the lower layer is an ester layer, and the lower layer of ester layer solution is sent to a nitrogen protection extractant evaporation device (8); after distilling and separating lithium chloride from the upper alcohol layer solution, partially refluxing and injecting alcohol liquid into a feed inlet of the crude distillation kettle assembly (1);
(3) filling sufficient nitrogen into the nitrogen protection extractant evaporation device (8) to discharge air, setting heating reflux time to be 3.5-4 h, and collecting a fraction at a temperature of 68-70 ℃ to obtain prepurified trimethyl borate;
(4) sending the prepurified trimethyl borate obtained in the step (3) into a prefabricated fraction detection device (9), and sending the qualified prepurified trimethyl borate into a triple nitrogen protection rectifying kettle component (7) for rectification if the purity of the trimethyl borate is not lower than 99.9%;
s4: rectifying
(1) Putting qualified prepurified trimethyl borate obtained in the step S3 and the step (4) into a 1-stage rectifying tower in a triple nitrogen protection rectifying still assembly (7), heating by an oil bath partition wall, enabling gas phase to escape to a tower plate, opening a rectifying product collecting valve and a storage tank valve after a plurality of condensation and vaporization processes, introducing trimethyl borate into the 1-stage rectifying product storage tank, opening a 1-stage rectifying product storage tank discharging valve and a rectifying tower continuous feeding regulating valve, and continuously feeding and producing;
(2) putting the grade 1 rectification product into a grade 2 rectification tower, repeating the step (1), introducing trimethyl borate into a grade 2 rectification product storage tank, opening a discharging valve of the grade 2 rectification product storage tank and a continuous feeding regulating valve of the rectification tower, and continuously feeding for production;
(3) putting the 2-level rectification product into a 3-level rectification tower, repeating the step (1), and introducing trimethyl borate into a 2-level rectification product storage tank to obtain the required electronic-level trimethyl borate;
s5: detection of
(1) Detecting the electronic grade trimethyl borate obtained in the step (3) in the step S4, wherein the purity of the main fraction trimethyl borate is required to be not lower than 99.99 percent, and entering a trace impurity detection program if the purity is qualified;
(2) detecting trace impurities in the electronic grade trimethyl borate in the step S4, wherein the total content of the impurities is required to be not higher than 0.0000005% (8.5N), and entering a packaging program if the total content of the impurities is qualified;
the environment-friendly preparation equipment of the electronic grade trimethyl borate matched with the preparation method is provided with a raw material treatment assembly, a crude distillation kettle assembly (1), a pre-extraction assembly (4) and a triple nitrogen protection distillation kettle assembly (7) in the order from feeding to discharging; wherein a solid-liquid separation device (2) and a crude fraction detection device (3) are arranged between the crude distillation kettle assembly (1) and the pre-extraction assembly (4); a nitrogen protection extractant evaporating device (8) and a prefabricated fraction detecting device (9) are sequentially arranged between the pre-extraction component (4) and the triple nitrogen protection rectifying kettle component (7); the pre-extraction component is also provided with an upper layer extraction and delivery device which is matched with the feed inlet of the crude distillation kettle component (1); the crude distillation kettle component (1) and the triple nitrogen protection rectification kettle component (7) are both provided with a condensing device (5) and a reflux control device (6).
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