CN103044474A - Low temperature preparation method of boron trifluoride dimethyl carbonate complex compound - Google Patents
Low temperature preparation method of boron trifluoride dimethyl carbonate complex compound Download PDFInfo
- Publication number
- CN103044474A CN103044474A CN2012105946167A CN201210594616A CN103044474A CN 103044474 A CN103044474 A CN 103044474A CN 2012105946167 A CN2012105946167 A CN 2012105946167A CN 201210594616 A CN201210594616 A CN 201210594616A CN 103044474 A CN103044474 A CN 103044474A
- Authority
- CN
- China
- Prior art keywords
- reaction
- boron trifluoride
- low temperature
- dimethyl ester
- carbonic acid
- Prior art date
- 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.)
- Pending
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to a chemical engineering product, a boron trifluoride dimethyl carbonate complex compound, in particular relates to a low temperature preparation method of the boron trifluoride dimethyl carbonate complex compound. The preparation method comprises the following steps: in a gas generating container, using boric acid and anhydrous hydrofluoric acid as raw materials, dehydrating and generating boron trifluoride gas, and sulfur trioxide is used as an dehydrating agent; in a purification container, purifying the boron trifluoride gas generated through concentrated sulphuric acid; in a complexing container, performing a complexing reaction of the purified boron trifluoride gas and the dimethyl carbonate; and in a filter, cooling down and crystallizing the liquid reactant of the complexing reaction, and the solid gathered is the boron trifluoride dimethyl carbonate complex compound. The technical scheme provided by the invention enables the temperature of the gas generating reaction and complexing reaction to be close to the room temperature, decreases energy consumption during production process and is low-carbon and environment friendly; the production process is safer and more controllable; and the boron trifluoride dimethyl carbonate complex compound is a solid white crystal, wherein the content of boron trifluoride is 40-43 percent in weight and the property of the boron trifluoride is stable.
Description
Technical field
The invention belongs to the Chemicals boric carbonic acid dimethyl ester complex trifluoride, be specifically related to the low temperature preparation method of boric carbonic acid dimethyl ester complex trifluoride.
Background technology
Boron trifluoride complex is the very strong catalyzer of a kind of activity, can be used in the multiple organic synthesis, especially in cephalosporins antibacterials synthesis technique, owing to introduce the reaction times that boron trifluoride complex has namely shortened existing product, again the yield of existing product is significantly improved.The present cephalosporins of boric carbonic acid dimethyl ester complex trifluoride is the most effective catalyzer in the chemosynthesis process that transform the C3 position, uses safety, convenient, and environmentally safe.
The production technique of boric carbonic acid dimethyl ester complex trifluoride is at present:
Sulfuric acid, boric acid and hydrofluoric acid are carried out the gas making reaction at 90-150 ℃, reaction times 8-18 hour, generate boron triflouride gas; Then mix with methylcarbonate, carry out complex reaction, temperature of reaction is 40-80 ℃, and the time is 4-12 hour.Obtain the complexing mother liquor, then be cooled to 20-50 ℃ of crystallization, from the complexing mother liquor, collect solid crystal as product.Production process need to consume a large amount of steam and heat; Technology controlling and process is strict, and certain danger is arranged.
Summary of the invention
Technical problem to be solved by this invention is that gas making reaction and complex reaction all need to carry out under comparatively high temps, and energy consumption is large and dangerous high, in order to overcome above deficiency, provides a kind of low temperature preparation method of boric carbonic acid dimethyl ester complex trifluoride.
In order to solve the problems of the technologies described above, technical scheme of the present invention is: the low temperature preparation method of described boric carbonic acid dimethyl ester complex trifluoride may further comprise the steps:
1) gas making reaction: in the gas making container, take boric acid and anhydrous hydrofluoric acid as raw material, dehydration generates boron triflouride gas, and dewatering agent is sulphur trioxide;
2) purify: in the purification container, the boron triflouride gas that generates is purified through the vitriol oil;
3) complex reaction: in the complexing container, boron triflouride gas and methylcarbonate after purifying are carried out complex reaction;
4) crystallization is filtered: in the strainer, with the reaction solution cooling crystallization of complex reaction, collect solid and be the boric carbonic acid dimethyl ester complex trifluoride product.
Boric acid and anhydrous hydrofluoric acid Dehydration are reversible reaction for boron trifluoride, promote reaction to carry out by the sulphur trioxide dehydration, and anhydrous system has prevented the boron trifluoride chance water decomposition of generation, thereby has reduced temperature of reaction, has shortened the reaction times.
Further, in the step 1), derive by vacuumizing the boron trifluoride that will generate, vacuum tightness is 0.07-0.098MPa, reaches the purpose that promotes reaction forward to carry out and improve reaction yield.
Further, the temperature of reaction of the gas making of step 1) reaction is 18 ~ 48 ℃, and the reaction times is 4 ~ 15 hours, adopted strong dewatering agent sulphur trioxide, thus decrease temperature of reaction, shortened the reaction times, effectively reduce energy consumption of reaction, improved simultaneously processing safety.
Further, the concentration of the vitriol oil step 2) is 85 ~ 98%.
Further, step 2) in, gauge pressure is 0 ~ 0.5MPa, increase pressure is conducive to the impurity in the vitriol oil absorption boron trifluoride, improves product purity.
Further, the temperature of reaction of the complex reaction in the step 3) is 20 ~ 40 ℃, and the reaction times is 4 ~ 12 hours.
Further, step 3) and step 4) are carried out simultaneously, and reaction solution circulates between complexing container and strainer, and filter temperature hangs down 8 ~ 15 ℃ than the temperature of reaction of complex reaction.Cooling was hypersaturated state after reaction solution entered strainer, separate out the boric carbonic acid dimethyl ester complex trifluoride crystal, reaction solution behind the crystallization enters complexing kettle again can be further and the boron trifluoride complexing, by this working cycle, make methylcarbonate and boron trifluoride carry out to greatest extent complexing, by the repeatedly alternative high temperature complexing of complexing, energy consumption is lower, better effects if.
Further, the weight of material ratio is in the step 1): sulphur trioxide: boric acid: anhydrous hydrofluoric acid=4 ~ 12: 1 ~ 3: 1 ~ 3;
Further, the weight of material ratio is in the step 3): methylcarbonate: boron triflouride gas=6: 3 ~ 6.
Further, boron trifluoride content is 40 ~ 43wt% in the product that step 4) is collected, and farthest is conducive to client's use.
Technical scheme provided by the invention so that gas making reaction and complex reaction near room temperature, reduced the energy consumption of production process, low-carbon green environmental protection, production process more safety are controlled, the boric carbonic acid dimethyl ester complex trifluoride that obtains is white crystalline solid, boron trifluoride content 40 ~ 43wt% wherein, stable performance.
Embodiment
Below in conjunction with following examples the present invention is described in detail:
Embodiment 1
Sulphur trioxide, boric acid, anhydrous hydrofluoric acid are joined in the gas making still with 4: 1: 1 weight ratio, react under 18 ℃ of conditions, in 15 hours reaction times, vacuum pump vacuumizes the derivation boron triflouride gas, and vacuum tightness is 0.07MPa.
The boron triflouride gas of deriving enters the purification still of the vitriol oil that concentration 85% is housed and purifies, and purification kettle meter pressure power is 0.2MPa.
Boron triflouride gas after the purification enters complexing kettle, is filled with methylcarbonate in the complexing kettle, and the mass ratio of the boron triflouride gas that every still produces in the loading level of methylcarbonate and the gas making still is 6:3, and the complex reaction temperature is 20 ℃, and the reaction times is 4 hours.
Complex reaction liquid circulates in complexing kettle and strainer, and filter temperature is lower 8 ℃ than complexing kettle temperature, and reaction solution becomes supersaturated solution under this temperature, crystallize out; Reaction solution behind the crystallization is returned again further complexing in the complexing kettle, collect crystal and be the solid boric carbonic acid dimethyl ester complex trifluoride through the whizzer drying.Product is white crystal, and wherein boron trifluoride content is 40%.
The testing method of boron trifluoride content: take by weighing Sodium Fluoride 1.5g, in the crucible that dries to constant weight, put into electric heating dry bath case oven dry 3 hours, bake out temperature is 180 ℃, and accurately weighed is M1, adds three grades of water 15ml dissolvings, add again sample 0.5000 ± 0.0002g, accurately weighed is M2, and crucible is put into electric heating dry bath case oven dry 3 hours, and bake out temperature is 180 ℃.Take out to move in the moisture eliminator being cooled to room temperature, accurately taking by weighing weight is M3.
Calculation formula:
Content %=[(M3-M1)/M2] * 100%
In the formula: the empty crucible of M1-------, Sodium Fluoride weight g
The weight g of M2-------sample
The gross weight g of crucible after the M3-------drying
This content is converted into boric carbonic acid dimethyl ester complex trifluoride purity and is about 99.85%, and visible complexing degree is very high, and impurity seldom.
Embodiment 2
Sulphur trioxide, boric acid, anhydrous hydrofluoric acid are joined in the gas making still with 8: 1: 1 mass ratio, and reaction is 8 hours under 30 ℃ of conditions, generates boron triflouride gas.Vacuum pump vacuumizes the derivation boron triflouride gas, and vacuum tightness is 0.08MPa.
The boron triflouride gas of deriving enters the purification still of the vitriol oil that concentration 93% is housed and purifies, and purification kettle meter pressure power is 0.4MPa.
Boron triflouride gas after the purification enters complexing kettle, is filled with methylcarbonate in the complexing kettle, and the mass ratio of the boron triflouride gas that every still produces in the loading level of methylcarbonate and the gas making still is 6: 4, and the complex reaction temperature is 30 ℃, and the reaction times is 8 hours.
Filter temperature is lower than 10 ℃ of complex reaction temperature, all the other reference examples 1.Product is white crystal, and wherein boron trifluoride content is 42%.This content is converted into boric carbonic acid dimethyl ester complex trifluoride purity and is about 99.5%, and visible complexing degree is very high, and impurity seldom.
Embodiment 3
Sulphur trioxide, boric acid, anhydrous hydrofluoric acid are joined in the gas making still with 12: 2: 3 weight ratio, and reaction is 4 hours under 48 ℃ of conditions, generates boron triflouride gas.Vacuum pump vacuumizes the derivation boron triflouride gas, and vacuum tightness is 0.098MPa.
The boron triflouride gas of deriving enters the purification still of the vitriol oil that concentration 98% is housed and purifies, and purification kettle meter pressure power is 0.5MPa.
Boron triflouride gas after the purification enters complexing kettle, is filled with methylcarbonate in the complexing kettle, and the mass ratio of the boron triflouride gas that every still produces in the loading level of methylcarbonate and the gas making still is 6: 6, and the complex reaction temperature is 40 ℃, and the reaction times is 12 hours.
Filter temperature is lower than 15 ℃ of complex reaction temperature, all the other reference examples 1.Product is white crystal, and wherein boron trifluoride content is 43%.This content is converted into boric carbonic acid dimethyl ester complex trifluoride purity and is about 99.99%.
Claims (10)
1. the low temperature preparation method of a boric carbonic acid dimethyl ester complex trifluoride is characterized in that, may further comprise the steps:
1) gas making reaction: in the gas making container, take boric acid and anhydrous hydrofluoric acid as raw material, dehydration generates three and fluoridizes
Boron gas, dewatering agent are sulphur trioxide;
2) purify: in the purification container, the boron triflouride gas that generates is purified through the vitriol oil;
3) complex reaction: in the complexing container, boron triflouride gas and methylcarbonate after purifying are carried out network
Close reaction;
4) crystallization is filtered: in the strainer, with the reaction solution cooling crystallization of complex reaction, collect solid and be three
Boron fluoride carbonic acid dimethyl ester complex product.
2. the low temperature preparation method of described a kind of boric carbonic acid dimethyl ester complex trifluoride according to claim 1 is characterized in that, in the described step 1), derives by vacuumizing the boron trifluoride that will generate, and vacuum tightness is 0.07-0.098MPa.
3. the low temperature preparation method of described a kind of boric carbonic acid dimethyl ester complex trifluoride according to claim 1 is characterized in that, the temperature of reaction of the gas making reaction of described step 1) is 18 ~ 48 ℃, and the reaction times is 4 ~ 15 hours.
4. the low temperature preparation method of described a kind of boric carbonic acid dimethyl ester complex trifluoride according to claim 1 is characterized in that described step 2) described in the concentration of the vitriol oil be 85 ~ 98%.
5. the low temperature preparation method of described a kind of boric carbonic acid dimethyl ester complex trifluoride according to claim 1 is characterized in that described step 2) in, gauge pressure is 0 ~ 0.5MPa.
6. the low temperature preparation method of described a kind of boric carbonic acid dimethyl ester complex trifluoride according to claim 1 is characterized in that the temperature of reaction of the complex reaction in the described step 3) is 20 ~ 40 ℃, and the reaction times is 4 ~ 12 hours.
7. the low temperature preparation method of described a kind of boric carbonic acid dimethyl ester complex trifluoride according to claim 1, it is characterized in that, described step 3) and step 4) are carried out simultaneously, and reaction solution circulates between complexing container and strainer, and filter temperature hangs down 8 ~ 15 ℃ than the temperature of reaction of complex reaction.
8. the low temperature preparation method of described a kind of boric carbonic acid dimethyl ester complex trifluoride according to claim 1 is characterized in that the weight of material ratio is in the described step 1): sulphur trioxide: boric acid: hydrofluoric acid=4 ~ 12: 1 ~ 3: 1 ~ 3.
9. the low temperature preparation method of described a kind of boric carbonic acid dimethyl ester complex trifluoride according to claim 1 is characterized in that the weight of material ratio is in the described step 3): methylcarbonate: boron triflouride gas=6: 3 ~ 6.
10. the low temperature preparation method of described a kind of boric carbonic acid dimethyl ester complex trifluoride according to claim 1 is characterized in that, boron trifluoride content is 40 ~ 43wt% in the product that step 4) is collected.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105946167A CN103044474A (en) | 2012-12-31 | 2012-12-31 | Low temperature preparation method of boron trifluoride dimethyl carbonate complex compound |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105946167A CN103044474A (en) | 2012-12-31 | 2012-12-31 | Low temperature preparation method of boron trifluoride dimethyl carbonate complex compound |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103044474A true CN103044474A (en) | 2013-04-17 |
Family
ID=48057356
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012105946167A Pending CN103044474A (en) | 2012-12-31 | 2012-12-31 | Low temperature preparation method of boron trifluoride dimethyl carbonate complex compound |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103044474A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104355315A (en) * | 2014-10-21 | 2015-02-18 | 东营合益化工有限公司 | Method for co-production of propylene glycol during production of boron trifluoride |
| CN109503638A (en) * | 2018-12-20 | 2019-03-22 | 润泰化学南通有限公司 | A kind of boron trifluoride complex production technology |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1817886A (en) * | 2006-03-22 | 2006-08-16 | 黑龙江豪运经贸有限公司 | Production of boric carbonic acid dimethyl ester complex trifluoride |
| CN1876660A (en) * | 2006-07-12 | 2006-12-13 | 黑龙江豪运经贸有限公司 | Complexing method of boron trifluoride methylcarbonate complex |
| CN101525343A (en) * | 2009-04-23 | 2009-09-09 | 于志红 | Preparation method of boron trifluoride complex |
| CN101829601A (en) * | 2009-03-11 | 2010-09-15 | 于景东 | Method for preparing environmentally-friendly catalyst for producing cephalosporin |
-
2012
- 2012-12-31 CN CN2012105946167A patent/CN103044474A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1817886A (en) * | 2006-03-22 | 2006-08-16 | 黑龙江豪运经贸有限公司 | Production of boric carbonic acid dimethyl ester complex trifluoride |
| CN1876660A (en) * | 2006-07-12 | 2006-12-13 | 黑龙江豪运经贸有限公司 | Complexing method of boron trifluoride methylcarbonate complex |
| CN101829601A (en) * | 2009-03-11 | 2010-09-15 | 于景东 | Method for preparing environmentally-friendly catalyst for producing cephalosporin |
| CN101525343A (en) * | 2009-04-23 | 2009-09-09 | 于志红 | Preparation method of boron trifluoride complex |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104355315A (en) * | 2014-10-21 | 2015-02-18 | 东营合益化工有限公司 | Method for co-production of propylene glycol during production of boron trifluoride |
| CN104355315B (en) * | 2014-10-21 | 2016-08-24 | 东营合益化工有限公司 | A kind of method producing boron triflouride gas joint production of propylene glycol |
| CN109503638A (en) * | 2018-12-20 | 2019-03-22 | 润泰化学南通有限公司 | A kind of boron trifluoride complex production technology |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109232628B (en) | Method for synthesizing lithium difluoro (oxalato) borate by one-pot method | |
| CN103012454A (en) | Method for preparing solid boron trifluoride acetonitrile complex and application thereof | |
| CN104355967B (en) | The method of autocatalysis one-step synthesis high puring aluminium isopropoxide | |
| RU2591703C2 (en) | Method for preparation of 3,3-dimethylbutyraldehyde | |
| CN102659181A (en) | Method for preparing phosphotungstic heteropoly acid with Keggin structure | |
| CN103043684A (en) | Method for producing ammonium hydrogen fluoride by recovering fluorine in wet process phosphoric acid tail gas | |
| CN102774846A (en) | Method for producing enriched boric-10 acid from trifluoride-anisole complex and application thereof | |
| CN103991882A (en) | Method for preparing potassium fluoride by using fluoride in liquid phase of wet process phosphoric acid | |
| CN112979411A (en) | Process for preparing triphenylchloromethane | |
| CN104876248A (en) | Method for preparing potassium sulfate and co-producing ammonium chloride | |
| CN103073408A (en) | Preparation method of dichlorodiphenylene ether ketone | |
| CN102923713A (en) | Method for sanitary production of sodium fluosilicate | |
| CN103044474A (en) | Low temperature preparation method of boron trifluoride dimethyl carbonate complex compound | |
| CN104262390A (en) | Continuous production method of high-efficiency and low-toxicity pesticide-acephate | |
| CN103803622B (en) | A kind of by the method for Aluminum Chloride Hexahydrate Dehydration for Aluminum chloride anhydrous | |
| CN105330545B (en) | The method that triazine ring cyclization mother liquid bits mesoxalic acid is recycled using stannic chloride as catalyst | |
| CN102910638B (en) | Preparation method of anhydrous lithium metaborate | |
| CN102134078A (en) | Method for closed-loop production of silicon tetrafluoride by utilizing sulfuric acid and quartz sand | |
| CN104150500A (en) | Method for preparing boron-10 acid with boron-10 trifluoride | |
| CN112299453B (en) | Preparation method of high-purity lithium fluoride | |
| CN101891757B (en) | Preparation method of catalyst for producing cephalosporin | |
| CN103694118A (en) | Preparation method of trifluoroacetic acid ethyl ester and preparation method of intermediate of trifluoroacetic acid ethyl ester | |
| CN101774651A (en) | Method for preparing reagent cobalt chloride hexahydrate | |
| CN102464674B (en) | Preparation method of trichlorfon | |
| CN101260038B (en) | Method for purifying 3,4,5-trimethoxylbenzoic acid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C05 | Deemed withdrawal (patent law before 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130417 |