CN101412728A - System and process for preparing B-trichloro-borazole - Google Patents
System and process for preparing B-trichloro-borazole Download PDFInfo
- Publication number
- CN101412728A CN101412728A CNA200710059898XA CN200710059898A CN101412728A CN 101412728 A CN101412728 A CN 101412728A CN A200710059898X A CNA200710059898X A CN A200710059898XA CN 200710059898 A CN200710059898 A CN 200710059898A CN 101412728 A CN101412728 A CN 101412728A
- Authority
- CN
- China
- Prior art keywords
- borazole
- trichlorine
- reaction
- special
- boron trichloride
- 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
Images
Abstract
The invention relates to a full set of a special experiment system which is suitable and controllable in a temperature state, an airflow state, a reflowing state, time and other aspects and is used for preparing B- trichloride borazole which is a colorless acicular crystal and is easy to sublimate, and a set of improved experiment operation process for preparing B- trichloride borazole. The B- trichloride borazole is an important material for reducing borazole as a special material, is often used as an initial substance for substitution reaction of a borazole ring and is also an important material applied to the research of various inorganic group substituted elements.
Description
Technical field
Boron trichloride and ammonium chloride through the special test system, carry out the organic chemistry building-up reactions in the inert atmosphere of standard, under special experiment condition, prepare colourless acicular B-trichlorine borazole.
Background technology
B-trichlorine borazole is the critical materials of reduction important source material borazole, and often is used as the initial substance of borazole nucleus substitution; Be the important source material (as: B-melamine borazole, B-three cyanogen sulphur borazoles, B-three nitroxyl borazoles, B-trinitro-borazole) that is applied to various inorganic group substituted element researchs simultaneously.
U.S., method, the existing certain level of the research of day in the preparation of B-trichlorine borazole: by the compound (B of borazole and hydrogenchloride
3N
3H
63HCl) thermolysis prepares B-trichlorine borazole, boron trichloride and Monomethylamine and obtains corresponding borazole product, the Powdered ammonium chloride of exsiccant and boron trichloride gas deferred reaction under the exsiccant condition of nitrogen gas in 250 ℃ of prepared in reaction trimethylammoniums-N-B-trichlorine borazole, pyrolysis by ammonia and boron trichloride and prepare and add ammonium chloride in B-trichlorine borazole, the chlorobenzene and feed boron trichloride gas simultaneously and prepare B-trichlorine borazole or the like.Some of them prepare product and do not have the report of corresponding physicochemical property aspect, some preparations limit by experimental technique can't enlarge that production, its product yield of some preparation methods are too low, the employed experiment reagent toxicity of some preparation methods is bigger or the like.
The method that this patent proposes is to be raw material with boron trichloride, ammonium chloride, is reaction medium with the toluene solution, preparation B-trichlorine borazole in special experimental system, under certain experimental technique condition.
Crucial part of the present invention has 2 points: the one, and the experimental implementation system of the aspects such as controlled state of temperature, air-flow condition, reflux state and time that a whole set of is suitable; Two is the more perfect experimental implementation technology of a cover.
Summary of the invention
Boron trichloride and ammonium chloride are in the inert atmosphere of standard, under the temperature condition more than 100 ℃, low-temperature reactor, the central reaction district with certain temperature regulatory function and high-speed stirring function, low-temp reaction reflux through special prepare colourless needle-like B-trichlorine borazole by special technological process.B-trichlorine borazole molecule is made up of the six circumference rings that B and N alternately are connected, and has a chlorine on the B atom, has a hydrogen on the N atom; B-trichlorine borazole product can be preserved in specific solution over a long time.
Test principle:
With boron trichloride, ammonium chloride is raw material, is reaction medium with the toluene solution, at preparation trichlorine borazole more than 100 ℃, under the exsiccant condition of nitrogen gas.Reaction formula is as follows:
Boron trichloride is a kind of not flammable, poisonous, mordant liquified compressed gas that is stored in the gas cylinder, and meets moisture hydrolysis immediately.And B-trichlorine borazole is a kind of very easily clear crystal of distillation, meets very responsively with water and alcohols material, presents violent chemical reaction; With will emit hydrogenchloride after damp atmosphere contacts; When discharging a large amount of heat and generate boric acid, ammonium ion and chlorion with the water vigorous reaction.Its fusing point is 84 ℃ and very easily distillation, and B-trichlorine borazole is carrying out irreversible slowly thermolysis under 100 ℃ the condition surpassing, and discharges hydrogenchloride and generates the solid of non-volatility.B-trichlorine borazole at room temperature is stored in the pipe of sealing, can decompose behind the some months to produce a spot of non-volatility solid product.
Because the singularity of test raw material and test product itself should be carried out test under the inert atmosphere state of strictness and absolute anhydrous envrionment conditions, test conditions is very harsh.Therefore pilot system, test operation process all there is very strict requirement.
1, the preparation system of B-trichlorine borazole
The requirement of pilot system:
● low-temperature reactor-be mainly used in the processing to boron trichloride;
● have the central reaction district of certain temperature adjusting, high-speed stirring function;
● reaction reflux-make organic reaction more abundant
● gas drier
● the stopping property of organic reaction system
1. special condensation dropping funnel:
In the basic material of preparation trichlorine borazole, boron trichloride is a kind of not flammable, poisonous, mordant liquified compressed gas that is stored in the gas cylinder, and pressure store is its vapour pressure 4.9psig (70 ℉), meets moisture hydrolysis immediately.Boron trichloride fusing point (freezing point) is-161.4 ℉ (107.4 ℃), and boiling point is 54.5 ℉ (12.5 ℃).For boron trichloride and ammonium chloride can be reacted normally, need the gaseous state boron trichloride is transformed into liquid boron trichloride, and be dissolved in the reaction medium toluene solution.We have designed special condensation dropping funnel for this reason---and skin is to add the heat-eliminating medium cold zone, internal layer is the gas channel of particular design, make the one end connect boron trichloride gas, what come out from the other end water clock then is boron trichloride liquid, device can be controlled the liquid droping speed of liquid boron chloride simultaneously, guarantees the control of raw material dosage in the experimentation.See＜5〉＜6〉part of accompanying drawing.
2. central reaction district:
The reaction of boron trichloride and ammonium chloride is carried out in the toluene medium, must be heated the reflux temperature of toluene.React with ammonium chloride for boron trichloride is dissolved in the toluene solution, reaction is normally carried out, need heating unit; Placing the four-hole bottle on the heating unit is the central reaction zone, possesses functions such as temperature control, high-speed stirring simultaneously, satisfies the experiment condition in central reaction district.See accompanying drawing＜1〉parts such as＜2 〉.
3. react reflux:
For making reaction more fully stop the volatilization of boron trichloride gas simultaneously, use spherical condensation tube and special condensation dropping funnel anabolic reaction backflow part.Its effect is to make to fail complete reaction in the central reaction district and evaporate into the gasiform boron trichloride again under the hot conditions in central reaction district, effect through the reaction reflux, be that liquid is added in the toluene solution by gas reforming again, realize further reaction, make reaction more abundant, both reduce simultaneously the loss of boron trichloride, saved raw material again.Accompanying drawing＜5〉parts such as＜10 〉.
4. gas drier:
Since the singularity of test, to the shielding gas of testing circumstance---and nitrogen carries out drying treatment, promptly utilizes Calcium Chloride Powder Anhydrous, silica gel, molecular sieve etc. to carry out gas drying, the drying conditions of strict guarantee reaction environment.Accompanying drawing＜9 〉.
Sealing effectiveness to each junction of system all has the strict guarantee measure simultaneously.
Description of drawings
Accompanying drawing is the preparation system synoptic diagram of B-trichlorine borazole
Wherein: the special condensation dropping funnel of＜1〉heating jacket＜2〉central reaction district＜3〉stirring rod＜4〉agitator motor＜5〉＜6〉special minute device of air＜7〉spinner-type flowmeter＜8〉tetrafluoro spinner-type flowmeter＜9〉gas drier＜10〉spherical condensation tube＜11〉bending drying tube＜12〉thermometer
2, the preparation technology of B-trichlorine borazole:
Test is prepared:
Because the specific (special) requirements of this test---i.e. test must be carried out in the dry environment under the blanket of nitrogen, because of Preparation before this each test link all will strictly be tested by the test operation requirement. Concrete steps as Lower:
(1) all test reagents carry out drying, the batching operation of per step on request on request in the dry atmosphere operation of self-control Operate in the case.
(2) all to carry out drying processing before test apparatus and testing equipment use, and before test with in the experimental rig Pass into dried inert gas, carry out simultaneously certain dry processing that add.
(3) must in the protective atmosphere of drying, carry out all test operation processes, required with the guarantee test process Special environment condition.
Test operation technology:
(1), shifts to an earlier date 48 hours with the toluene drying, ammonium chloride was dried in baking oven in 24 hours in advance; Glass The glass vessel are dried in baking oven.
(2), press support reaction unit shown in the figure one, and pass in advance dried nitrogen, under heating state, advance Row system drying.
(3), in the dry atmosphere control box of self-control, prepare burden
(4), under nitrogen protection, add ammonium chloride and toluene, heat simultaneously and follow high-speed stirred until temperature Degree reaches the refluxing toluene temperature.
(5), utilize spinner flowmeter to control the boron chloride flow velocity, utilize special condensation dropping funel with tri-chlorination Boron gas changes into liquid and is dissolved in the toluene solution, makes it fully to react with ammonium chloride. Wherein special Add dry ice and acetone in the condensation dropping funel and realize that (control to liquid transformation by temperature by gaseous state for boron chloride About-77 ℃).
(6), the conditions such as each reagent dosage, reaction time of controlling react fully and carry out, and finally obtain the trichlorine borazole Toluene solution.
(7), the self-control dry atmosphere control box in the reactant suction filtration, obtain B-trichlorine borazole solution.
(8), the decompression rotary evaporation by 50--60 ℃, obtain B-trichlorine borazole crystal.
Embodiment
(1) anhydrous sodium sulphate of 48 hours 70g that weigh is dry 500ml toluene in advance.
(2) shift to an earlier date the 24 hours 60g ammonium chloride (choosing impurity) of weighing, 130 ℃ of dryings of carrying out 8--10 hour.
(3) the dry atmosphere operation box of self-control fed nitrogen in 24 hours in advance, puts into silica gel etc., performed corresponding seal operation.
(4) 4 hours supports are good in advance for experimental system, feed dried high pure nitrogen, carry out drying treatment under the condition of heating, perform the seal operation of each link.
(5) logical high pure nitrogen protection (80ml/s) before the experiment beginning.
(6) in the dry atmosphere operation box of self-control, fed general nitrogen protection in 30 minutes in advance after, filter toluene 500ml to beaker through B, toluene in the beaker is moved in the Erlenmeyer flask after in Erlenmeyer flask, filling general for a moment nitrogen, seal.
In the time of (7) 60 ℃, add ammonium chloride, toluene to four-hole bottle successively.
(8) open stirring, open spherical condensation tube water-cooled circulation, and heater switch transferred to preset the temperature place.
(9) thermometer heating registration is about 112 ℃, when refluxing toluene is arranged, adds dry ice and acetone and regulate temperature in the special condensation dropping funnel outside special condensation dropping funnel, feeds boron trichloride afterwards.(the under meter registration is about 60ml/s) notes the time.
(10) experimentation notes observing boron trichloride dropping state and reflux state, notices that nitrogen flow rate changes.
After (11) 10 hours, experiment is finished.
(12) the self-control dry atmosphere operation box in the reactant pumping rate, obtain purified liquid reaction solution.
(13) the decompression rotary evaporation by 50--60 ℃ obtains B-trichlorine borazole.
Claims (2)
1, the present invention relates to prepare the special experimental system of a whole set of suitable aspect such as controlled state of temperature, air-flow condition, reflux state and time of B-trichlorine borazole.
2, the present invention relates to prepare the more perfect experimental implementation technology of a cover of B-trichlorine borazole.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200710059898XA CN101412728A (en) | 2007-10-17 | 2007-10-17 | System and process for preparing B-trichloro-borazole |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200710059898XA CN101412728A (en) | 2007-10-17 | 2007-10-17 | System and process for preparing B-trichloro-borazole |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101412728A true CN101412728A (en) | 2009-04-22 |
Family
ID=40593492
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA200710059898XA Pending CN101412728A (en) | 2007-10-17 | 2007-10-17 | System and process for preparing B-trichloro-borazole |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101412728A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110064448A (en) * | 2019-05-17 | 2019-07-30 | 山东新希望六和集团有限公司 | One kind is for being saponified reflux nitrogen filled protection device |
| CN112375094A (en) * | 2020-11-25 | 2021-02-19 | 中国人民解放军国防科技大学 | Catalyst-free high-yield synthesis method and device for trichloroborazine |
-
2007
- 2007-10-17 CN CNA200710059898XA patent/CN101412728A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110064448A (en) * | 2019-05-17 | 2019-07-30 | 山东新希望六和集团有限公司 | One kind is for being saponified reflux nitrogen filled protection device |
| CN112375094A (en) * | 2020-11-25 | 2021-02-19 | 中国人民解放军国防科技大学 | Catalyst-free high-yield synthesis method and device for trichloroborazine |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Watts et al. | Morphology control in high yield boron carbide | |
| CN101412728A (en) | System and process for preparing B-trichloro-borazole | |
| CN114105157B (en) | Double-temperature-zone dense-tube synthesis technology of boron arsenide powder material | |
| Choi et al. | The sulphur cycle in cement kilns: vapour pressures and solid-phase stability of the sulphate phases | |
| Pet’kov et al. | Characterization and controlling thermal expansion of materials with kosnarite-and langbeinite-type structures | |
| CN104588046B (en) | Method for preparing BiOCl by using choline chloride/urea low-melting-point eutectic solvent as burning agent | |
| Depci et al. | Comparison of different synthesis methods to produce lithium triborate and their effects on its thermoluminescent property | |
| Hanf et al. | High-temperature hydrolysis of sodium chloride | |
| CN101597269B (en) | Method for synthesizing tebuthiuron raw medicine | |
| Hart et al. | The synthesis of new calcium borate compounds by hydrothermal methods | |
| Weinmann et al. | Towards continuous processes for the synthesis of precursors of amorphous Si/B/N/C ceramics | |
| Smirnova et al. | Phase Formation in the MgO–B2O3–P2O5 System | |
| CN206362178U (en) | A kind of vacuum synthesis stove | |
| Chtioui et al. | Crystal structure, thermal analysis and IR spectroscopic investigation of (C6H9N2) H2XO4 (X= As, P) | |
| CN101717279A (en) | Method for producing agricultural potassium metaphosphate | |
| Pagano et al. | Single‐Crystal Structure Determination and Solid‐State NMR Investigations of Lithium Nitridosilicate Li2SiN2 Synthesized by a Precursor Approach Employing Amorphous “Si (CN2) 2” | |
| CN1271077C (en) | Method for preparing-trichloro sucrose-6-ethyl ester | |
| US5659078A (en) | Process for the preparation of trichloroacetyl chloride | |
| Arceo et al. | Fluxing reactions of sulfates and carbonates in cement clinkering II. The system CaCO3K2CO3 | |
| CN101602773B (en) | Method for preparing biethyl diacid lithium borate | |
| Oueslati-Omrani et al. | Standard Formation Enthalpy of Na 2 O–ZnO–P 2 O 5 Series Glasses | |
| US3279891A (en) | Apparatus for production of fine-crystalline boron phosphide | |
| Solntsev et al. | Raman scattering study of crystalline and melting states of BaO· 2B2O3 | |
| CN108285130A (en) | A kind of preparation method and detection method of lithium borohydride | |
| CN101885492B (en) | Preparation method of sodium tetraborate as pH standard reagent |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20090422 |