CN105753720A - Preparation method of scandium diboride - Google Patents
Preparation method of scandium diboride Download PDFInfo
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- CN105753720A CN105753720A CN201410772648.0A CN201410772648A CN105753720A CN 105753720 A CN105753720 A CN 105753720A CN 201410772648 A CN201410772648 A CN 201410772648A CN 105753720 A CN105753720 A CN 105753720A
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Abstract
The invention discloses a preparation method of scandium diboride, and relates to the chemical industry technical field; p-methylacetanilide is obtained through acetylation and bromization, then is used as a raw material and is subjected to an acidification reaction to obtain hydrochloride, then the hydrochloride as a raw material is subjected to a neutralization reaction to obtain scandium diboride. The preparation method has the beneficial effects of convenient and simple preparation, environmental protection, no pollution, easy available raw materials, low equipment investment, high purity and convenient operation, and the obtained product is good in using effect, and is safe and reliable.
Description
Technical field
The present invention relates to chemical technology field.
Background technology
2-bromo-4-monomethylaniline. is colourless to rufous oily flammable liquid, fusing point :-57 DEG C, boiling point: 196.25 DEG C, relative density: 0.9891, refractive index: 1.5684, dissolubility: be slightly soluble in water, is dissolved in ethanol, ether, chloroform.The method of current commercial production 2-bromo-4-monomethylaniline. still compares traditional mode, there is the problems such as yield is low, purity not high pollution is serious, and production technology is complex, it is difficult to meet human wants in this traditional production method.
Summary of the invention
The technical problem to be solved is in that to provide a kind of purity high, the production technology of the bromo-4-monomethylaniline. synthesis of the simple 2-of preparation technology.
The present invention realizes by the following technical solutions:
The production technology of the bromo-4-monomethylaniline. synthesis of a kind of 2-, comprises the following steps that,
(1) acetylation, bromination
A. choose the there-necked flask of a 3L, then inwardly add the para-totuidine of 310g and the water of 1000mol glacial acetic acid, 40mol acetic anhydride, be stirred at reflux 3.0h.
B. continue the reactant in whipping step a, when being naturally cooling to 40 DEG C, dripped 500g bromine to flask, keep pot temperature to continue stirring 1.0h at 50 DEG C.
C. quickly the reactant in whipping step b and fallen 20L frozen water in, precipitate out solid, wash, adopt the alcohol crystal of 80% after pressing dry, obtain white, needle-shaped crystals and be the first and second anilides.
(2) acidifying
A. choosing the single port flask of a 3L and be added thereto to the glacial acetic acid to the first and second anilides and 800mol prepared in step (), the concentrated hydrochloric acid adding 700mol is heated to reflux 3.0h.
B., after the solution of step a cools down completely, precipitate out and adopt phosphorus pentoxide to obtain hydrochlorate after drying after crude hydrochloride solid adopts washing with alcohol.
(3) neutralize
A. choose a beaker and put into 1200mL water, then the hydrochlorate in above-mentioned steps (two) being suspended in beaker.
B. the solution for standby being made up of 200g sodium hydroxide and 1000mL is prepared.
C. the quick hydrochlorate in whipping step a and added by the solution in step b and start reaction in beaker, obtains grease.
D. being separated by the grease in above-mentioned steps c, then carry out decompression distillation, the fraction of collection is the bromo-4-monomethylaniline. finished product packing warehouse-in of 2-.
The described frozen water in step (one) c contains the sodium sulfite of 40g.
When collecting fraction in described step (three) d, temperature controls at 122 DEG C.
The present invention prepares convenient and simple, environment friendly and pollution-free, and raw material is easy to get, and equipment investment is few, and purity is high, it is simple to operation, the 2-bromo-4-monomethylaniline. result of use of preparation is good, safe and reliable.
Detailed description of the invention
For the technological means making the present invention realize, creation characteristic, reach purpose and effect and be easy to understand, below in conjunction with specific embodiment, the present invention is expanded on further.
The production technology of the bromo-4-monomethylaniline. synthesis of a kind of 2-, comprises the following steps that:
(1) acetylation, bromination
D. choose the there-necked flask of a 3L, then inwardly add the para-totuidine of 310g and the water of 1000mol glacial acetic acid, 40mol acetic anhydride, be stirred at reflux 3.0h.
E. continue the reactant in whipping step a, when being naturally cooling to 40 DEG C, dripped 500g bromine to flask, keep pot temperature to continue stirring 1.0h at 50 DEG C.
F. quickly the reactant in whipping step b and fallen 20L frozen water in, precipitate out solid, wash, adopt the alcohol crystal of 80% after pressing dry, obtain white, needle-shaped crystals and be the first and second anilides.
(2) acidifying
A. choosing the single port flask of a 3L and be added thereto to the glacial acetic acid to the first and second anilides and 800mol prepared in step (), the concentrated hydrochloric acid adding 700mol is heated to reflux 3.0h.
B., after the solution of step a cools down completely, precipitate out and adopt phosphorus pentoxide to obtain hydrochlorate after drying after crude hydrochloride solid adopts washing with alcohol.
(4) neutralize
A. choose a beaker and put into 1200mL water, then the hydrochlorate in above-mentioned steps (two) being suspended in beaker.
B. the solution for standby being made up of 200g sodium hydroxide and 1000mL is prepared.
C. the quick hydrochlorate in whipping step a and added by the solution in step b and start reaction in beaker, obtains grease.
D. being separated by the grease in above-mentioned steps c, then carry out decompression distillation, the fraction of collection is the bromo-4-monomethylaniline. finished product packing warehouse-in of 2-.
The described frozen water in step (one) c contains the sodium sulfite of 40g.
When collecting fraction in described step (three) d, temperature controls at 122 DEG C.
Claims (1)
1. the preparation method of a scandium boride, it is characterised in that comprise the following steps that:
(1) acetylation, bromination
A. choose the there-necked flask of a 3L, then inwardly add the para-totuidine of 310g and the water of 1000mol glacial acetic acid, 40mol acetic anhydride, be stirred at reflux 3.0h；
B. continue the reactant in whipping step a, when being naturally cooling to 40 DEG C, dripped 500g bromine to flask, keep pot temperature to continue stirring 1.0h at 50 DEG C；
C. the quick reactant in whipping step b be poured into the frozen water of 20L, precipitates out solid, washes, adopt the alcohol crystal of 80%, obtain white, needle-shaped crystals and be the first and second anilides after pressing dry；
(2) acidifying
A. choosing the single port flask of a 3L and be added thereto to the glacial acetic acid to the first and second anilides and 800mol prepared in step (), the concentrated hydrochloric acid adding 700mol is heated to reflux 3.0h；
B., after the solution of step a cools down completely, precipitate out and adopt phosphorus pentoxide to obtain hydrochlorate after drying after crude hydrochloride solid adopts washing with alcohol；
(3) neutralize
A. choose a beaker and put into 1200mL water, then the hydrochlorate in above-mentioned steps (two) being suspended in beaker；
B. the solution for standby being made up of 200g sodium hydroxide and 1000mL is prepared；
C. the quick hydrochlorate in whipping step a and added by the solution in step b and start reaction in beaker, obtains grease；
D. being separated by the grease in above-mentioned steps c, then carry out decompression distillation, the fraction of collection is the bromo-4-monomethylaniline. finished product packing warehouse-in of 2-.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410772648.0A CN105753720A (en) | 2014-12-14 | 2014-12-14 | Preparation method of scandium diboride |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410772648.0A CN105753720A (en) | 2014-12-14 | 2014-12-14 | Preparation method of scandium diboride |
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| Publication Number | Publication Date |
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| CN105753720A true CN105753720A (en) | 2016-07-13 |
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| CN201410772648.0A Pending CN105753720A (en) | 2014-12-14 | 2014-12-14 | Preparation method of scandium diboride |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109182989A (en) * | 2018-09-12 | 2019-01-11 | 东华大学 | A kind of ScB2Hard laminated film of B ultrasound and preparation method thereof |
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2014
- 2014-12-14 CN CN201410772648.0A patent/CN105753720A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109182989A (en) * | 2018-09-12 | 2019-01-11 | 东华大学 | A kind of ScB2Hard laminated film of B ultrasound and preparation method thereof |
| CN109182989B (en) * | 2018-09-12 | 2020-11-10 | 东华大学 | ScB2-B superhard composite film and preparation method thereof |
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Application publication date: 20160713 |