CN102311305A - Immersed adsorption method for preparing environmentally friendly carbon tetrachloride - Google Patents
Immersed adsorption method for preparing environmentally friendly carbon tetrachloride Download PDFInfo
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- CN102311305A CN102311305A CN201110238402A CN201110238402A CN102311305A CN 102311305 A CN102311305 A CN 102311305A CN 201110238402 A CN201110238402 A CN 201110238402A CN 201110238402 A CN201110238402 A CN 201110238402A CN 102311305 A CN102311305 A CN 102311305A
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- China
- Prior art keywords
- carbon tetrachloride
- environmentally friendly
- tetracol phenixin
- preparation
- environmental protection
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- 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.)
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- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
Abstract
The invention relates to a preparation method of environmentally friendly carbon tetrachloride. The preparation method comprises the following steps: putting high quality active carbon of 40 meshes in a cylindrical glass column for several times according to a case of 20-25kg each time, wherein the bottom of the circular glass column is provided with a stop valve, and a little amount of glass wool separates the upper part of the stop valve and active carbon; and throwing industrial carbon tetrachloride into an elevated tank, transferring to the circular glass column to fully exchange the industrial carbon tetrachloride with active carbon, and repeating for two times to reach the environmentally friendly carbon tetrachloride. The adsorption method for preparing environmentally friendly carbon tetrachloride, which has the advantages of simple operation, economic serviceability, less investment, low cost, easily available equipment, and short production period, is suitable for industrialization.
Description
Technical field
The invention belongs to the organic solvent field, be specifically related to a kind of preparation method of environmental protection level tetracol phenixin.
Background technology
Tetracol phenixin is a kind of organic solvent (CCl commonly used
4Mol 153.82), at organic synthesis, chemical analysis, scientific research and education, industrial production and fire-fighting domain purposes is extremely widely arranged.Owing to the attention of various countries to environmental protection and atmosphere and ozonosphere protection, some chemistry and industrial chemicals that diminish environment were obtaining strict control in the last few years.The restriction tetracol phenixin uses to be paid attention to specially.But tetracol phenixin plays not replaceable vital role in environmental protection is analyzed just, has obtained extensive approval, prepares highly purified environmental protection level tetracol phenixin and is used for environmental monitoring and demonstrates particularly important.
The tetracol phenixin of industry is constantly to be replaced by chlorine by dithiocarbonic anhydride to form, so, in finished product, tend to residual a small amount of dithiocarbonic anhydride, methylene dichloride, trichloromethane and methylene derivatives.As prepare the fine tetracol phenixin and just must remove above-mentioned impurity.Usual method is fully to react with potassium hydroxide-ethanol solution earlier, washs to remove two keys and methylene derivatives with oxygenant then.
Summary of the invention
The purpose of this invention is to provide a kind of novel method of environmental protection level tetracol phenixin preparation, promptly utilize active carbon adsorption to prepare environmental protection level tetracol phenixin.
The technical scheme that realizes the object of the invention is following:
A kind of preparation method of environmental protection level tetracol phenixin is characterized in that comprising the steps:
(1) the cylindrical glass post is put in 40 order high grade activated carbon gradation, each 20-25 kilogram, pipe valve is arranged at the glass cylinder bottom, has a small amount of glass wool to separate between pipe valve top and the gac;
(2) the technical grade tetracol phenixin is squeezed into header tank, relay in the glass cylinder again, itself and gac are fully exchanged, absorption reaches the environmental protection level repeatedly for twice.
Advantage of the present invention and beneficial effect are:
The present invention utilizes active carbon adsorption to prepare environmental protection level tetracol phenixin, compares with other method to have great advantage, and this method is very easily operated, and is economic and practical, less investment, and cost is low, and equipment is easy to get, and is with short production cycle, and market is comparatively wide.
Embodiment
Below in conjunction with specific embodiments the present invention is further specified,, can not limit protection scope of the present invention with following illustrating to help understanding content of the present invention.
Embodiment 1:
(1) 40 order high grade activated carbons are put into the cylindrical glass post, each 20-25 kilogram, pipe valve is arranged at this glass cylinder bottom, has a small amount of glass wool to separate-the glass wool sealing coat between pipe valve top and the gac.
(2) will detect qualified technical grade tetracol phenixin and squeeze into header tank, relay in the right cylinder again.Itself and gac are fully soaked, have reached absorption, exchange, emit heat this moment, heavy putting after 48 hours carried out infrared detection, in impurely greatly reduce.Can reach environmental protection level effect repeatedly for twice.
The ir spectra absorbance measurement
3030
cm-1 2960
cm-1 2930
m-1
≤0.03≤0.03≤0.03 (what meaning? Need do and specify)
Packing instructions are extremely strict, need the polytetrafluoroethylene membrane sealing, keep in Dark Place.
Key problem in technology and discussion
(1) selection of raw material and gac is very important, and he influences the quality of result and product.
(2) header tank is reinforced can avoid the human injury, and exchange absorption is more complete, accelerates reaction time.
(3) the entire operation process must ventilate, be lower than under the room temperature and carry out, and tetracol phenixin is volatile, is prone to human body is damaged.
Claims (1)
1. the preparation method of an environmental protection level tetracol phenixin is characterized in that: comprise the steps:
(1) the cylindrical glass post is put in 40 order gac gradation, each 20-25 kilogram, pipe valve is arranged at the glass cylinder bottom, has a small amount of glass wool to separate between pipe valve top and the gac;
(2) the technical grade tetracol phenixin is squeezed into header tank, relay in the glass cylinder again, itself and gac are fully soaked, exchange, absorption reaches the environmental protection level repeatedly for twice.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110238402A CN102311305A (en) | 2011-08-19 | 2011-08-19 | Immersed adsorption method for preparing environmentally friendly carbon tetrachloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110238402A CN102311305A (en) | 2011-08-19 | 2011-08-19 | Immersed adsorption method for preparing environmentally friendly carbon tetrachloride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102311305A true CN102311305A (en) | 2012-01-11 |
Family
ID=45424913
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110238402A Pending CN102311305A (en) | 2011-08-19 | 2011-08-19 | Immersed adsorption method for preparing environmentally friendly carbon tetrachloride |
Country Status (1)
| Country | Link |
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| CN (1) | CN102311305A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105646138A (en) * | 2014-11-26 | 2016-06-08 | 天津市科密欧化学试剂有限公司 | Preparation method of chromatographic-grade carbon tetrachloride |
| CN105693461A (en) * | 2014-11-26 | 2016-06-22 | 天津市科密欧化学试剂有限公司 | Preparation method of chromatographic grade dichloromethane |
| CN105693462A (en) * | 2014-11-26 | 2016-06-22 | 天津市科密欧化学试剂有限公司 | Preparation method of chromatographic grade trichloromethane |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3631116A (en) * | 1968-01-12 | 1971-12-28 | Lothar Hornig | Process for the manufacture of carbon tetrachloride |
| CN2379461Y (en) * | 1999-07-25 | 2000-05-24 | 杨吉兴 | Equipment for purifying carbon tetrachloride |
| CN1327952A (en) * | 2001-06-02 | 2001-12-26 | 吉林大学 | Equipment for purifying extractant of mineral oil in water and process for treating adsorbent |
| CN2573497Y (en) * | 2002-09-20 | 2003-09-17 | 史永刚 | Adsorption column for purifying carbon tetrachloride |
| CN102267864A (en) * | 2011-08-09 | 2011-12-07 | 天津市化学试剂研究所 | Preparation method of chromatographic-grade carbon tetrachloride |
-
2011
- 2011-08-19 CN CN201110238402A patent/CN102311305A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3631116A (en) * | 1968-01-12 | 1971-12-28 | Lothar Hornig | Process for the manufacture of carbon tetrachloride |
| CN2379461Y (en) * | 1999-07-25 | 2000-05-24 | 杨吉兴 | Equipment for purifying carbon tetrachloride |
| CN1327952A (en) * | 2001-06-02 | 2001-12-26 | 吉林大学 | Equipment for purifying extractant of mineral oil in water and process for treating adsorbent |
| CN2573497Y (en) * | 2002-09-20 | 2003-09-17 | 史永刚 | Adsorption column for purifying carbon tetrachloride |
| CN102267864A (en) * | 2011-08-09 | 2011-12-07 | 天津市化学试剂研究所 | Preparation method of chromatographic-grade carbon tetrachloride |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105646138A (en) * | 2014-11-26 | 2016-06-08 | 天津市科密欧化学试剂有限公司 | Preparation method of chromatographic-grade carbon tetrachloride |
| CN105693461A (en) * | 2014-11-26 | 2016-06-22 | 天津市科密欧化学试剂有限公司 | Preparation method of chromatographic grade dichloromethane |
| CN105693462A (en) * | 2014-11-26 | 2016-06-22 | 天津市科密欧化学试剂有限公司 | Preparation method of chromatographic grade trichloromethane |
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Application publication date: 20120111 |