Preparation method and device of trimethyl borate-10

A technology of trimethyl borate and esterification reaction, applied in the field of trimethyl boron-10 acid, can solve the problems of large loss of trimethyl borate, difficulty in single treatment, complicated process, etc. Beautiful, good separation effect

Inactive Publication Date: 2014-01-22

TIANJIN UNIV +1

2 Cites 4 Cited by

AI-Extracted Technical Summary

Problems solved by technology

[0006] Wu Changmei, Liaoning Research Institute of Chemical Industry, published an article in 2000, using industrial boron trifluoride-10 ether complex as raw material, using calcium chloride as defluorinating agent, using methanol as the medium for reaction, and adding quantitative catalyst to prepare boron-10 The process of acid produces trimethyl boron-10 acid, but the loss of trimethyl borate during the distillation process is relatively large

[0007] Patent CN102774846A provides a boron trifluoride-anisole complex as the main raw material in the process of producing boron-10 acid, which also needs to go through the step of generating trimethyl boron-10 acid. The process of this method is relatively complicated. The equipment requires very good airtightness, and the side reaction products are various mixtures, which are difficult ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine

Method used

(a) reaction unit is purged 5~10min with high-purity nitrogen, avoids the interference of moisture in the air;

(c) rectifying tower head tank enters extraction agent N,N-dimethylformamide or dimethyl sulfoxide or mixed extraction agent, before entering extraction agent, extraction agent is suitably heated to 30~55 ℃ , can reduce the time to reach stable operation in the tower;

This method can be used for industrial continuous production, and the extraction effect of extraction agent is better, and production capacity is stronger, and two kinds of extraction agents are re...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine

Abstract

The invention relates to a preparation method and device of trimethyl borate-10. The preparation method comprises the steps of adding reactants into a reaction kettle, taking methanol as a solvent, and stirring for reacting for 30-45h; setting the reaction temperature to be 50-70 DEG C, and performing esterification reaction to generate trimethyl borate-10; performing azeotropic distillation on an esterification reaction product, and setting the temperature to be 70-90 DEG C; collecting a fraction at the temperature of 50-60 DEG C, then continuously heating, and recovering methanol; adding the fraction collected in azeotropic distillation into an extraction and distillation tower kettle; heating the tower kettle, controlling the heating voltage to be 120-150V and controlling the total reflux time to be 20-30min according to the total reflux speed to meet a heat load of a system, adding an extraction agent N, N-dimethylformamide or dimethyl sulfoxide or a mixed extraction agent into a high-level tank at the tower top of a distillation tower, and collecting trimethyl borate at the temperature of 67-68.5 DEG C at the tower top. The operation of the method is stable, and the purity of trimethyl borate-10 obtained by the method can be above 99%.

Application Domain

Group 3/13 element organic compoundsBoron-oxygen compounds +1

Technology Topic

Dimethyl formamideChemistry +11

Image

Examples

Experimental program(3)

Example Embodiment

[0067] Example 1

[0068] 1 Esterification reaction

[0069] (a) Purge the reaction kettle with high-purity nitrogen for 5-10 minutes, and adjust the reactants in a molar ratio 10 BF 3 :CaCl 2 :CH 3 The ratio of ONa=1:1.5:3.0 is added to the reactor, and methanol is used as the solvent to make the raw materials evenly distributed in it, which is conducive to stirring. Turn on the stirring device and set the speed to about 150r/min;

[0070] (b) Set the reaction temperature to 70°C and the reaction time to 30h;

[0071] 2 azeotropic distillation

[0072] (a) The reaction product is subjected to azeotropic distillation at a temperature of 70°C;

[0073] (b) Collect 50-60°C fractions, then continue to increase the temperature, recover methanol, and recycle.

[0074] 3 Extractive distillation

[0075] (a) Put the distillate into the extractive distillation tower kettle, turn on the 6 heating pack power supply and 1 condensate water switch. In order to ensure the heat transfer performance of the tower body, the tower body is insulated with 5 insulation tapes and refluxed for 30 minutes;

[0076] (b) Add the extractant N,N-dimethylformamide from the 4 high-position tank on the top of the tower, and heat the extractant to 30°C before entering the extractant to prevent the temperature from being too low and the tower will not easily achieve stable operation;

[0077] (c) When the temperature meter at the top of the tower 2 reaches 67℃, start to collect the fractions. Use the 3 reflux ratio controller to adjust the reflux ratio to 3:1. Collect the fractions at 67~68℃ to obtain trimethyl boron-10 acid The purity is 98.45%;

[0078] This method can be used for industrial continuous production, with relatively strong production capacity, stable operation, high purity of the product obtained, and the product can be directly applied: for welding, no additional solvent is added, which improves productivity; it can prepare boron-10 Acid, used in the nuclear industry.

Example Embodiment

[0079] Example 2

[0080] 1 Esterification reaction

[0081] (a) Purge the reactor with high-purity nitrogen for about 5 to 10 minutes, and adjust the reactants to the molar ratio of the reactants 10 BF 3 :CaCl 2 :CH 3 The ratio of ONa=1:1.7:3.4 is added to the reactor, and methanol is used as the solvent to make the raw materials evenly distributed in it, which is good for stirring. Turn on the stirring device and set the speed to about 200r/min;

[0082] (b) Set the reaction temperature to 60°C and the reaction time to 35h.

[0083] 2 azeotropic distillation

[0084] (a) The reaction product is subjected to azeotropic distillation, and the temperature is set to 80°C;

[0085] (b) Collect 50-60°C fractions, then continue to increase the temperature, recover methanol, and recycle.

[0086] 3 Extractive distillation

[0087] (a) Add the distillate to the extractive distillation tower kettle, turn on the 6 heating pack power supply and 1 condensate water switch. In order to ensure the heat transfer performance of the tower body, the tower body is insulated with 5 insulation tapes, and the total reflux is about 30 minutes;

[0088] (b) The top of the tower enters the extractant dimethyl sulfoxide from the 4 high-position tank, and the extractant is heated to 45°C before entering the extractant to prevent the temperature from being too low and it is difficult to achieve stable operation in the tower;

[0089] (c) When the temperature meter at the top of the tower reaches 67℃, start collecting fractions. Collect the 67~68.5℃ fractions. Use the 3 reflux ratio controller to adjust the reflux ratio of 0.5 to extract the fractions. The purity of trimethyl boron-10 acid is measured. Is 99.29%.

[0090] This method can be used in industrial continuous production, with relatively strong production capacity, stable operation, high purity of the product obtained, and the product can be directly applied: used in the manufacture of paraffin, resin, petroleum solvents, ketone catalysts, and also used in the electronics industry Wait. For welding, no additional solvent is added to improve productivity; boron-10 acid can be prepared for use in the nuclear industry; used as a doping source for semiconductors and the preparation of high-purity boron.

Example Embodiment

[0091] Example 3

[0092] 1 Esterification reaction

[0093] (a) Purge the reactor with high-purity nitrogen for about 5 to 10 minutes, and adjust the reactants to the molar ratio of the reactants 10 BF 3 :CaCl 2 :CH 3 The ratio of ONa=1:1.8:3.6 is added to the reactor, and methanol is used as the solvent to make the raw materials evenly distributed in it, which is good for stirring. Turn on the stirring device and set the speed to about 300r/min;

[0094] (b) Set the reaction temperature to 50°C and the reaction time to 45h;

[0095] 2 azeotropic distillation

[0096] (a) The reaction product is subjected to azeotropic distillation at a temperature of 90°C,

[0097] (b) Collect 50-60°C fractions, then continue to increase the temperature, recover methanol, and recycle.

[0098] 3 Extractive distillation

[0099] (a) Put the distillate into the extractive distillation tower kettle, turn on the 6 heating pack power supply and 1 condensate water switch. In order to ensure the heat transfer performance of the tower body, the tower body is insulated with 5 insulation tapes, and the total reflux is about 25 minutes;

[0100] (b) The top of the tower enters the mixed extractant of the extractant dimethyl sulfoxide and N,N-dimethylformamide from the 4 high position tank, and the extractant is heated to 55℃ before entering the extractant to prevent the temperature from being too low and the inside of the tower is difficult Achieve stable operation;

[0101] (c) When the temperature meter at the top of the tower 2 has stabilized, start to collect the fractions. Collect the fractions at a temperature of about 67.5-68.5℃. Use the 3 reflux ratio controller to adjust the reflux ratio 2:1 to extract the fractions and determine the component content, boron-10 The purity of trimethyl acid was measured to be 99.05%;

[0102] This method can be used in industrial continuous production. The extraction effect of the extractant is relatively good, and the production capacity is relatively strong. When the extractant is recycled, the two extractants are recovered separately, the operation is stable, the product purity is relatively high, and the product can be directly applied : Used in the manufacture of paraffin, resin, petroleum solvent, ketone catalyst, and also used in the electronics industry. For welding, it improves the technical requirements of productivity, air tightness and mechanical strength of the weld; it can prepare high-purity boron-10 acid for nuclear industry; it can be used in military equipment metal materials by adding boron-10 To the shielding effect of radiation protection.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine

Login to view more

PUM

Description & Claims & Application Information

We can also present the details of the Description, Claims and Application information to help users get a comprehensive understanding of the technical details of the patent, such as background art, summary of invention, brief description of drawings, description of embodiments, and other original content. On the other hand, users can also determine the specific scope of protection of the technology through the list of claims; as well as understand the changes in the life cycle of the technology with the presentation of the patent timeline. Login to view more.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine

Login to view more

Classification and recommendation of technical efficacy words

Good separation effect
Strong production capacity

Preparation method and device of trimethyl borate-10

A technology of trimethyl borate and esterification reaction, applied in the field of trimethyl boron-10 acid, can solve the problems of large loss of trimethyl borate, difficulty in single treatment, complicated process, etc. Beautiful, good separation effect

AI-Extracted Technical Summary

Problems solved by technology

Method used

Abstract

Image

Examples

Example Embodiment

Example Embodiment

Example Embodiment

PUM

Description & Claims & Application Information

Similar technology patents

Polyester fiber enhanced breadth and high-performance polyvinyl chloride composite material and preparation thereof

Novel rotary roller drying machine

Clean and effective preparation of oligoxylose

Cross-laminated wood processing equipment

Device and method for recovering cooling liquid for machining

Classification and recommendation of technical efficacy words

Vacuum packaging method for symmetric hot rolling manufactured stainless steel clad plates

High COD, high ammonia nitrogen and high salinity industrial wastewater treatment method

Multi-layer oil-water separator and working method therefor

Method for separating and purifying erythritol from fermentation liquor

System and method for separating and removing circulating tumor cell and blood platelet in blood

Cross-laminated wood processing equipment

Polyester fiber enhanced breadth and high-performance polyvinyl chloride composite material and preparation thereof

Clean and effective preparation of oligoxylose

Novel rotary roller drying machine