CN107337219A - A kind of preparation method of infrared light spectrum level KBr - Google Patents
A kind of preparation method of infrared light spectrum level KBr Download PDFInfo
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- CN107337219A CN107337219A CN201710699228.8A CN201710699228A CN107337219A CN 107337219 A CN107337219 A CN 107337219A CN 201710699228 A CN201710699228 A CN 201710699228A CN 107337219 A CN107337219 A CN 107337219A
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- kbr
- spectrum level
- infrared light
- light spectrum
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/14—Purification
- C01D3/18—Purification with selective solvents
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/10—Bromides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/14—Purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A kind of preparation method of infrared light spectrum level KBr of the present invention, it is characterised in that put into KBr raw material in organic solvent, ultrasonic irradiation shakes 6~8h, and decompression filters, and press dry filter cake；Filter cake is put into deionized water, is uniformly mixed, is filtered；Filtrate is slowly added into refining agent in batches, further freezing and crystallizing；After solidliquid mixture is filtered under diminished pressure into separation, crystal is washed with refining agent, filter cake is pressed dry, vacuum drying, that is, obtains infrared spectrum level KBr, and nitrogen protection is lower to be encapsulated.The present invention refines purification, effectively removes the high impurity of middle infrared absorption of raw material by the deep purifying to common specification KBr; its is easy to operate, is not related to chemical reaction process, and production cost is low; it is a kind of green method for preparing infrared light spectrum level KBr suitable for large-scale production.
Description
Technical field
The present invention relates to a kind of preparation method of order of spectrum special agent, more particularly to a kind of infrared light spectrum level KBr
Preparation method.
Background technology
KBr is colourless crystallization or white powder, has strong saline taste, sees photochromic flavescence, has certain hygroscopicity.Bromination
Potassium is widely used in medical, daily-use chemical industry etc., is pharmaceutically used as lithographic printing ink and spy as nerous sedative, daily chemical industry
Kind soap compound, Light sensitive materials industry are used to manufacture photographic film, developer, egative film intensifier, toner and color picture bleaching
Agent etc..KBr is used as infrared spectrum sample test carrier, KBr in an important application of modern analysis scientific domain
Tabletting is to prepare the main method of the infrared sample of solid, and order of spectrum KBr is the essential special examination of infrared spectrum analysis
Agent.Commercially available common bromination potassium content meets or exceeds the pure standard of analysis, but still suffers from the high impurity of micro infrared absorption, in
Infrared region (4000-400cm-1) absorption is opaque, and infrared spectrum when related impurities strong absorption band is to sample test produces serious
Interference, can not meet related science development test requirement.
Spectrographic laboratory 2011,28 (5), 2590 disclose complexation-crystallization roasting technique method, obtain infrared spectrum analysis and use
KBr.The introducing of wherein ethylenediamine tetra-acetic acid (EDTA) makes complex process, not only adds production cost while 700 DEG C of height
Temperature roasting, high energy consumption, is not suitable for large-scale production.With the development of the applied science such as China's medicine, chemical industry, material, to infrared
The demand of order of spectrum KBr is increasing, especially the industry such as scientific research, colleges and universities, inspection detection.Infrared light spectrum level KBr
Price is high, studies infrared light spectrum level KBr process, is not only worth with Important Economic, while to meeting that Domestic Scientific Research is given birth to
The Special use demand to KBr special agent is produced, it is significant.
The content of the invention
Problem to be solved by this invention is to provide a kind of preparation method of infrared light spectrum level KBr, and it is not related to chemistry
Reaction, energy consumption is low, simple process, production cost are low, easily accomplishes scale production.
In order to solve the above problems, the invention provides a kind of preparation method of infrared light spectrum level KBr, its feature exists
In, including step in detail below：
The first step：Under room temperature condition, KBr raw material is put into organic solvent, the quality of organic solvent and KBr
Than for 3: 1~5: 1, ultrasonic irradiation shakes 6~8h, at 20~60 DEG C, decompression filters temperature control, press dry filter cake；
Second step：The filter cake that the first step is obtained is put into deionized water, is heated to 90~100 DEG C, is stirred
It is even, filtered while hot after continuously stirring 30~60 minutes；
3rd step：Filtrate obtained by second step is slowly added into refining agent in batches, gained mixture continue stirring 30~
After 60 minutes, stand to room temperature, one-step freezing of going forward side by side crystallization, 10~12h is incubated at 2~8 DEG C；
4th step：After the solidliquid mixture that 3rd step obtains is filtered under diminished pressure into separation, crystal, filter cake pressure are washed with refining agent
It is dry, 4~6h is dried in vacuo at 100~150 DEG C, that is, obtains infrared spectrum level KBr, nitrogen protection is lower to be encapsulated.
Preferably, the purity of KBr raw material is 99% in the first step.
Preferably, the organic solvent in the first step be acetone the aqueous solution, water: the mass ratio of acetone be 1: 10~1:
20。
Preferably, the mass ratio of KBr raw material is 1: 1~3 in the dosage and the first step of deionized water in the second step
∶2。
Preferably, the refining agent in the 3rd step, the 4th step is tetrahydrofuran.
Preferably, the mass ratio of KBr is 1: 5~4: 5 in the dosage and the first step of the refining agent in the 3rd step.
It is raw materials used commercially available in the present invention.
Compared with prior art, the beneficial effects of the present invention are：
1st, the present invention program is refined purification, effectively removed in raw material by the deep purifying to common specification KBr
The high impurity of infrared absorption, obtain infrared light spectrum level KBr, there is provided the common specification raw material of a utilization directly prepares infrared light
The effective way of spectrum level KBr；
2nd, process proposed by the present invention, it is easy to operate, it is not related to chemical reaction process, production cost is low, suitable for rule
Modelling produces, and is a kind of green method for preparing infrared light spectrum level KBr.
Brief description of the drawings
Fig. 1 is the infrared spectrum comparison diagram of KBr infrared spectrum and KBr raw material prepared by the purification of embodiment 2；Its
In, KBr-A is KBr raw material, and KBr-B is the KBr of purified preparation.
Embodiment
To become apparent the present invention, hereby with preferred embodiment, it is described in detail below.
Embodiment
A kind of preparation method of infrared light spectrum level KBr：
The first step：Under room temperature condition, by the KBr raw material 500g of purity 99% put into acetone soln (deionized water:
Acetone quality ratio is 1: 20 solution prepared) in, the mass ratio of acetone soln and KBr raw material is 3: 1, ultrasonic irradiation shake
6h is swung, at 20~60 DEG C, decompression filters temperature control, press dry filter cake；
Second step：The filter cake that the first step is obtained is put into 500mL deionized waters, and electric jacket is heated to 90 DEG C, stirring
It is well mixed, carry out heat filtering after continuously stirring 30 minutes；
3rd step：Filtrate obtained by second step is slowly added into 100mL tetrahydrofurans in batches, gained mixture continues to stir
After mixing 60 minutes, stand to room temperature, one-step freezing of going forward side by side crystallization, 2~8 DEG C of insulation 10h；
4th step：The solidliquid mixture that 3rd step obtains is filtered under diminished pressure separation, with ice-cold (the about 0 DEG C) tetrahydrofurans of 50mL
Crystal is washed, filter cake press dry, and 100 DEG C of vacuum drying 4h, obtains infrared light spectrum level KBr finished product 310g, nitrogen protection packaging.
Embodiment 2
A kind of preparation method of infrared light spectrum level KBr：
The first step：Under room temperature condition, by the KBr raw material 1500g of purity 99% put into acetone soln (deionized water:
Acetone quality ratio is 1: 10 solution prepared) in, the mass ratio of acetone soln and KBr raw material is 5: 1, ultrasonic irradiation shake
8h is swung, at 20~60 DEG C, decompression filters temperature control, press dry filter cake；
Second step：The filter cake that the first step is obtained is put into 2250mL deionized waters, and electric jacket is heated to 100 DEG C, stirs
Mix well mixed, heat filtering is carried out after continuously stirring 60 minutes；
3rd step：Filtrate obtained by second step is slowly added into 1200mL tetrahydrofurans in batches, gained mixture continues
After stirring 30 minutes, stand to room temperature, one-step freezing of going forward side by side crystallization, 2~8 DEG C of insulation 12h；
4th step：The solidliquid mixture that 3rd step obtains is filtered under diminished pressure separation, with ice-cold (about 0 DEG C) the tetrahydrochysene furans of 240mL
Mutter and wash crystal, filter cake press dry, and 150 DEG C of vacuum drying 6h, obtains infrared light spectrum level KBr finished product 960g, nitrogen tamper seal
Dress.
Under same experimental conditions, the KBr (bromination of KBr raw material (KBr-A) and purified preparation is done respectively
Potassium-B) infrared spectrum, comparison diagram is as shown in Figure 1.The infrared spectrogram of KBr raw material is in 1579.50cm-1、1380.07cm-1、
1111.03cm-1、614.59cm-1There are obvious impurity peaks, particularly 3420.28cm in place-1There is a very strong Impurity Absorption band.And pass through
The KBr infrared spectrum prepared is purified, above-mentioned Impurity Absorption band is almost wholly absent, and only small fluctuation, spectrogram is almost
For a straight line, show that the KBr purity of purified preparation is very high, absorption is transparent, complies fully with infrared light spectrum level bromination
Potassium reagent requirement.
Claims (6)
1. a kind of preparation method of infrared light spectrum level KBr, it is characterised in that including step in detail below：
The first step：Under room temperature condition, KBr raw material is put into organic solvent, the mass ratio of organic solvent and KBr is
3: 1~5: 1, ultrasonic irradiation shakes 6~8h, and at 20~60 DEG C, decompression filters temperature control, press dry filter cake；
Second step：The filter cake that the first step is obtained is put into deionized water, is heated to 90~100 DEG C, is uniformly mixed, even
Continuous stirring is filtered while hot after 30~60 minutes；
3rd step：Filtrate obtained by second step is slowly added into refining agent in batches, gained mixture continues 30~60 points of stirring
Zhong Hou, stand to room temperature, one-step freezing of going forward side by side crystallization, 10~12h is incubated at 2~8 DEG C；
4th step：After the solidliquid mixture that 3rd step obtains is filtered under diminished pressure into separation, crystal is washed with refining agent, filter cake press dry,
4~6h is dried in vacuo at 100~150 DEG C, that is, obtains infrared spectrum level KBr, nitrogen protection is lower to be encapsulated.
2. the preparation method of infrared light spectrum level KBr as claimed in claim 1, it is characterised in that bromination in the first step
The purity of potassium raw material is 99%.
3. the preparation method of infrared light spectrum level KBr as claimed in claim 1, it is characterised in that having in the first step
Machine solvent be acetone the aqueous solution, water：The mass ratio of acetone is 1: 10~1: 20.
4. the preparation method of infrared light spectrum level KBr as claimed in claim 1, it is characterised in that gone in the second step from
The mass ratio of KBr raw material is 1: 1~3: 2 in the dosage and the first step of sub- water.
5. the preparation method of infrared light spectrum level KBr as claimed in claim 1, it is characterised in that the 3rd step, the 4th
Refining agent in step is tetrahydrofuran.
6. the preparation method of the infrared light spectrum level KBr as described in claim 1 or 5, it is characterised in that in the 3rd step
Refining agent dosage and the first step in KBr mass ratio be 1: 5~4: 5.
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| CN201710699228.8A CN107337219B (en) | 2017-08-15 | 2017-08-15 | A kind of preparation method of infrared light spectrum level potassium bromide |
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| CN201710699228.8A CN107337219B (en) | 2017-08-15 | 2017-08-15 | A kind of preparation method of infrared light spectrum level potassium bromide |
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| CN107337219A true CN107337219A (en) | 2017-11-10 |
| CN107337219B CN107337219B (en) | 2019-05-17 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108394917A (en) * | 2018-03-05 | 2018-08-14 | 刘燕廷 | One kind containing 6-apa, Amoxicillin, benzylpenicillin potassium work salt spectroscopic pure potassium bromide recoverying and utilizing method |
| CN109437245A (en) * | 2018-12-14 | 2019-03-08 | 山东金城晖瑞环保科技有限公司 | The method of organic solvent Isolating chlorinated sodium and sodium bromide |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104512914A (en) * | 2013-09-26 | 2015-04-15 | 天津市光复科技发展有限公司 | Production method of KBr namely dedicated carrier of infrared spectrum |
| CN205575666U (en) * | 2016-04-26 | 2016-09-14 | 天津市光复精细化工研究所 | Special carrier potassium bromide preparation facilities of infrared spectrum |
-
2017
- 2017-08-15 CN CN201710699228.8A patent/CN107337219B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104512914A (en) * | 2013-09-26 | 2015-04-15 | 天津市光复科技发展有限公司 | Production method of KBr namely dedicated carrier of infrared spectrum |
| CN205575666U (en) * | 2016-04-26 | 2016-09-14 | 天津市光复精细化工研究所 | Special carrier potassium bromide preparation facilities of infrared spectrum |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108394917A (en) * | 2018-03-05 | 2018-08-14 | 刘燕廷 | One kind containing 6-apa, Amoxicillin, benzylpenicillin potassium work salt spectroscopic pure potassium bromide recoverying and utilizing method |
| CN109437245A (en) * | 2018-12-14 | 2019-03-08 | 山东金城晖瑞环保科技有限公司 | The method of organic solvent Isolating chlorinated sodium and sodium bromide |
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| Publication number | Publication date |
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| CN107337219B (en) | 2019-05-17 |
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