CN109908617A - A kind of purification of specpure reagent tetrachloro-ethylene, packing, storage method - Google Patents
A kind of purification of specpure reagent tetrachloro-ethylene, packing, storage method Download PDFInfo
- Publication number
- CN109908617A CN109908617A CN201910287744.9A CN201910287744A CN109908617A CN 109908617 A CN109908617 A CN 109908617A CN 201910287744 A CN201910287744 A CN 201910287744A CN 109908617 A CN109908617 A CN 109908617A
- Authority
- CN
- China
- Prior art keywords
- tetrachloro
- ethylene
- packing
- glove box
- purification
- 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
- CYTYCFOTNPOANT-UHFFFAOYSA-N Perchloroethylene Chemical group ClC(Cl)=C(Cl)Cl CYTYCFOTNPOANT-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 229950011008 tetrachloroethylene Drugs 0.000 title claims abstract description 47
- 238000012856 packing Methods 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000003860 storage Methods 0.000 title claims abstract description 20
- 239000003153 chemical reaction reagent Substances 0.000 title claims abstract description 15
- 238000000746 purification Methods 0.000 title claims abstract description 15
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 36
- 229910052757 nitrogen Inorganic materials 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 238000010926 purge Methods 0.000 claims description 7
- 239000002131 composite material Substances 0.000 claims description 6
- 239000012629 purifying agent Substances 0.000 claims description 6
- 229920003023 plastic Polymers 0.000 claims description 5
- 239000004033 plastic Substances 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- 238000011017 operating method Methods 0.000 claims description 3
- 125000006850 spacer group Chemical group 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000009833 condensation Methods 0.000 claims 1
- 230000005494 condensation Effects 0.000 claims 1
- 238000012432 intermediate storage Methods 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 238000004821 distillation Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 238000004134 energy conservation Methods 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 239000007789 gas Substances 0.000 description 6
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 6
- 239000000391 magnesium silicate Substances 0.000 description 6
- 229910052919 magnesium silicate Inorganic materials 0.000 description 6
- 235000019792 magnesium silicate Nutrition 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 239000003463 adsorbent Substances 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 239000002808 molecular sieve Substances 0.000 description 5
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 5
- 239000002699 waste material Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 238000006386 neutralization reaction Methods 0.000 description 4
- 238000005457 optimization Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- NRZWYNLTFLDQQX-UHFFFAOYSA-N p-tert-Amylphenol Chemical compound CCC(C)(C)C1=CC=C(O)C=C1 NRZWYNLTFLDQQX-UHFFFAOYSA-N 0.000 description 2
- 230000007420 reactivation Effects 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- YNJBWRMUSHSURL-UHFFFAOYSA-N trichloroacetic acid Chemical compound OC(=O)C(Cl)(Cl)Cl YNJBWRMUSHSURL-UHFFFAOYSA-N 0.000 description 2
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- QCDYQQDYXPDABM-UHFFFAOYSA-N phloroglucinol Chemical compound OC1=CC(O)=CC(O)=C1 QCDYQQDYXPDABM-UHFFFAOYSA-N 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of purifications of specpure reagent tetrachloro-ethylene, packing, storage method, including neutralizing distillation still, the right side for neutralizing destilling tower connects pipe bundle condenser, the bottom of the pipe bundle condenser is equipped with hold-up vessel, the pipe bundle condenser is connected to the hold-up vessel, the first pump of right side connection of the hold-up vessel, the right side termination of first pump connects rectifying column, the right side connection circulation pipe bundle condenser of the rectifying column, the bottom of the circulation pipe bundle condenser is connected to pan tank, the second pump of right side connection of the pan tank, the right side of second pump connects pressurized keg, the right side of the pressurized keg connects glove box.Entirety cost of material of the present invention is low, and it is less with blowdown to consume energy, whole more energy conservation and environmental protection.
Description
Technical field
The present invention relates to chemical industry manufacture technology field, specially a kind of purification, packing, the storage of specpure reagent tetrachloro-ethylene
Deposit method.
Background technique
Tetrachloro-ethylene is a kind of important organic solvent, and the production industry with cleaning, industrial refrigeration agent is widely applied.Due to
Tetrachloro-ethylene has stronger extracting power to lipoid material, and physicochemical property is very close with carbon tetrachloride, and environmental pollution
It is small, so HJ637-2018 " the measurement infrared spectrophotometry of water-quality petroleum and vegetable and animals oils " standard is by it as carbon tetrachloride
Best substitute.It is required according to HJ637-2018-5.3, tetrachloro-ethylene substitution carbon tetrachloride must satisfy " to dry 4cm sky stone
English cuvette is reference, in 2800cm-1~3100cm-1Between using 4cm quartz colorimetric utensil measure tetrachloro-ethylene, 2930cm-1,
2960cm-1,3030cm-10.34,0.07,0 " should be no more than respectively by locating absorbance.
Presently commercially available tetrachloro-ethylene analytical reagents, in 2930cm after infrared scan-1,2960cm-1, place has relatively strong
Absorption peak, be not able to satisfy HJ637-2018-5.3 requirement.Leading to the underproof main cause of infrared absorbency is tetrachloro-ethylene
Inside be added to stabilizer p-tert-amylphenol and homologue, in addition there are also tetrachloro-ethylene is light-exposed, water, oxygen decompose generate it is micro
Trichloroacetic acid and hydrogen chloride.Conventional method of purification has magnesium silicate, active carbon adsorption, atmospheric and vacuum distillation method at present.According to
The four steps absorption that application publication number CN108083973A is used, a step rectification method purified, and processing step is more, energy consumption compared with
Greatly, yield is not high.The magnesium silicate regeneration of absorption needs Muffle furnace high temperature sintering;Active carbon, regenerating molecular sieve can generate largely
Exhaust gas, waste liquid, the feasibility of industrialized production is lower.
According to application publication number CN107778130A use the absorption of 13X molecular sieve, activated carbon adsorption, adsorption of magnesium silicate, three
Walk absorption method.Cause tetrachloro-ethylene be not able to satisfy HJ637-2018-5.3 require due to be impurity p-tert-amylphenol and
Homologue, trichloroacetic acid, hydrogen chloride.And active carbon, magnesium silicate, 13X molecular sieve be not high to its adsorptive selectivity, and technical grade
Unstability between tetrachloro-ethylene batch.Refining effect is difficult to meet HJ637-2018-5.3 requirement, and the regeneration of adsorbent is equally deposited
The CN108083973A the problem of.
Presently commercially available environmentally friendly grade, order of spectrum Zellon shelf-life are generally shorter, such as Tianjin loftily environmentally friendly grade four
6 months clear shelf-lifves of vinyl chloride.The reason for causing the tetrachloro-ethylene shelf-life not grown is mainly that interiors of products introduces moisture content, water
Part will lead to the decomposition of tetrachloro-ethylene.Moisture content mainly from packing container sealing performance, before packing container clean performance,
For the above, then how to invent a kind of purification of specpure reagent tetrachloro-ethylene, packing, storage method, this becomes
Our problems to be solved.
Summary of the invention
The purpose of the present invention is to provide a kind of purifications of specpure reagent tetrachloro-ethylene, packing, storage method, solve
The problem of proposed in background technique.
To solve the above problems, the invention provides the following technical scheme: a kind of purification of specpure reagent tetrachloro-ethylene, point
Dress, storage method, including distillation still is neutralized, the right side for neutralizing destilling tower connects pipe bundle condenser, the pipe bundle condenser
Bottom be equipped with hold-up vessel, the pipe bundle condenser is connected to the hold-up vessel, the right side connection first of the hold-up vessel
Pump, the right side termination of first pump connect rectifying column, the right side connection circulation pipe bundle condenser of the rectifying column, the circulation
The bottom connection pan tank of pipe bundle condenser, the second pump of right side connection of the pan tank, the right side connection of second pump add
Bucket is pressed, the right side of the pressurized keg connects glove box.
As present invention further optimization mode, the inside of the glove box is equipped with packing pipeline, the packing pipeline
It is connect with packing small bottle container.
As present invention further optimization mode, following operating procedure is specifically included, S1 takes 1000g technical grade tetrachloro
Ethylene adds 10g composite purifying agent, heats infinite reflux 30 minutes, and temperature is controlled at 120~125 DEG C, directly steams after reflux;
S2, the tetrachloro-ethylene that S1 is distilled out move into rectifying column, discard front and back fraction 1~5%, collect middle distillate;
S3 moves into S2 finished product in the pressurized keg with nitrogen protection, and pressurized keg purges 30 points with drying nitrogen using preceding
Clock;After pressurized keg fills finished product tetrachloro-ethylene, add nitrogen protection.It is placed on warehouse or its fixed-site.
S4, by the vial of packing with pure water 3~5 times, 105 DEG C of drying boxes continuous drying two hours are moved into
Nitrogen purges 30 minutes in -25 DEG C of dew point glove boxes below;
Pressurized keg equipped with tetrachloro-ethylene is accessed in glove box with pipeline, is dispensed in glove box by S5, keeps gloves
- 25 DEG C of dew point or less of case;
The tetrachloro-ethylene dispensed is added Tetrafluoro spacer, bottle cover for locking, removes glove box, put up label, vacuum plastic by S6
Envelope.
In step S1, the composite purifying agent is set as natrium carbonicum calcinatum: sodium hydroxide: anhydrous sodium sulfate=1:1:1 mass
Compare mixture.
It further include after pressurized keg fills tetrachloro-ethylene finished product, directly moving into as present invention further optimization mode
Warehouse storage when needing to dispense, is connect with pipeline with glove box.
As present invention further optimization mode, the glove box is purged using preceding with nitrogen, -25 DEG C of dewpoint requirements with
Under.
Compared with prior art, beneficial effects of the present invention are as follows:
The method of the present invention is avoided without using adsorbents such as magnesium silicate, active carbon, molecular sieves due to adsorbent reactivation generation
Exhaust gas, waste liquid, waste residue, using nitrogen purging container, outside air, moisture content has been isolated to product matter in vacuum plastic sealing pack container
Amount influences, and extends shelf life of products, purifying technique neutralization, two step of rectifying, technique is relatively easy, and production process only has a small amount of consolidate
It is useless to generate.
Detailed description of the invention
Fig. 1 is present invention production storage facilities easy structure schematic diagram;
Fig. 2 is dispensing apparatus structural schematic diagram of the present invention;
Fig. 3 is tetrachloro-ethylene infrared detection comparison result schematic diagram of the invention;
Fig. 4 is tetrachloro-ethylene technical grade gas chromatogram of the invention;
Fig. 5 is tetrachloro-ethylene alkali neutralization gas chromatogram of the invention;
Fig. 6 is rectifying gas chromatogram schematic diagram after tetrachloro-ethylene alkali neutralization of the invention.
In figure: neutralizing destilling tower -1, pipe bundle condenser -2, hold-up vessel -3, the first pump -4, rectifying column -5, circulation tubulation
Condenser -6, pan tank -7, the second pump -8, pressurized keg -9, glove box -10, storage bottle -11, nitrogen storage tank -12.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Please refer to Fig. 1-6, this practical invention provides a kind of technical solution: a kind of purification of specpure reagent tetrachloro-ethylene,
Packing, storage method, including destilling tower 1 is neutralized, the right side for neutralizing destilling tower 1 connects pipe bundle condenser 2, and the tubulation is cold
The bottom of condenser 2 is equipped with hold-up vessel 3, and the pipe bundle condenser 2 is connected to the hold-up vessel 3, the right side of the hold-up vessel 3
The first pump 4 of connection, the right side termination of first pump 4 are connected to rectifying column 5, and the right side connection circulation tubulation of the rectifying column 5 is cold
Condenser 6, the bottom of the circulation pipe bundle condenser 6 are connected to pan tank 7, and the second pump 8 of right side connection of the pan tank 7 is described
The right side of second pump 8 connects pressurized keg 9, and the right side of the pressurized keg 9 connects glove box 10.
The inside of the glove box 10 is equipped with packing pipeline 11, and the packing pipeline 11 is connect with packing small bottle container 12.
Following operating procedure is specifically included, S1 takes 1000g technical grade tetrachloro-ethylene to add the heating of 10g composite purifying agent is complete to return
Stream 30 minutes, temperature are controlled at 120~125 DEG C, are directly steamed after reflux;
S2, the tetrachloro-ethylene that S1 is distilled out move into rectifying column, discard front and back fraction 1~5%, collect middle distillate;
S3 moves into S2 finished product in the pressurized keg with nitrogen protection, and pressurized keg purges 30 points with drying nitrogen using preceding
Clock;After pressurized keg fills finished product tetrachloro-ethylene, add nitrogen protection.It is placed on warehouse or its fixed-site.
S4, by the vial of packing with pure water 3~5 times, 105 DEG C of drying boxes continuous drying two hours are moved into
Nitrogen purges 30 minutes in -25 DEG C of dew point glove boxes below;
Pressurized keg equipped with tetrachloro-ethylene is accessed in glove box with pipeline, is dispensed in glove box by S5, keeps gloves
- 25 DEG C of dew point or less of case;
The tetrachloro-ethylene dispensed is added Tetrafluoro spacer, bottle cover for locking, removes glove box, put up label, vacuum plastic by S6
Envelope.
In step S1, the composite purifying agent is set as natrium carbonicum calcinatum: sodium hydroxide: anhydrous sodium sulfate=1:1:1 mass
Compare mixture.
Further include after pressurized keg fills tetrachloro-ethylene finished product, directly moving into warehouse storage, when needing to dispense, with pipeline with
Glove box connection.
The glove box is purged using preceding with nitrogen, and -25 DEG C of dewpoint requirements or less.
To sum up, the method for the present invention is avoided without using adsorbents such as magnesium silicate, active carbon, molecular sieves due to adsorbent reactivation
Exhaust gas, waste liquid, the waste residue of generation, using nitrogen purging container, outside air, moisture content pair has been isolated in vacuum plastic sealing pack container
Product quality influences, and extends shelf life of products, purifying technique neutralization, two step of rectifying, technique is relatively easy, and production process is only few
The solid waste of amount generates.
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention, for this field skill
For art personnel, it is clear that invention is not limited to the details of the above exemplary embodiments, and without departing substantially from spirit of the invention or
In the case where essential characteristic, the present invention can be realized in other specific forms.Therefore, in all respects, should all incite somebody to action
Embodiment regards exemplary as, and is non-limiting, the scope of the present invention by appended claims rather than on state
Bright restriction, it is intended that including all changes that fall within the meaning and scope of the equivalent elements of the claims in the present invention
It is interior.Any reference signs in the claims should not be construed as limiting the involved claims.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (6)
1. a kind of purification of specpure reagent tetrachloro-ethylene, packing, storage method, including destilling tower (1) is neutralized, feature exists
In: the right side for neutralizing destilling tower (1) connects pipe bundle condenser (2), and the bottom of the pipe bundle condenser (2) is equipped with intermediate storage
Slot (3), the pipe bundle condenser (2) are connected to the hold-up vessel (3), the first pump of right side connection of the hold-up vessel (3)
(4), the right side termination of first pump (4) is connected to rectifying column (5), the right side connection circulation tubulation condensation of the rectifying column (5)
The bottom of device (6), circulation pipe bundle condenser (6) is connected to pan tank (7), the second pump of right side connection of the pan tank (7)
(8), the right side of second pump (8) connects pressurized keg (9), and the right side of the pressurized keg (9) connects glove box (10).
2. purification, the packing, storage method of a kind of specpure reagent tetrachloro-ethylene according to claim 1, feature exist
In: the inside of the glove box (10) is equipped with packing pipeline (11), and the packing pipeline (11) and packing small bottle container (12) are even
It connects.
3. purification, the packing, storage method of a kind of specpure reagent tetrachloro-ethylene according to claim 1, feature exist
In: following operating procedure is specifically included, S1 takes 1000g technical grade tetrachloro-ethylene that the heating infinite reflux 30 of 10g composite purifying agent is added to divide
Clock, temperature are controlled at 120~125 DEG C, are directly steamed after reflux;
S2, the tetrachloro-ethylene that S1 is distilled out move into rectifying column, discard front and back fraction 1~5%, collect middle distillate;
S3 moves into S2 finished product in the pressurized keg with nitrogen protection, and pressurized keg is purged 30 minutes using preceding with drying nitrogen;Add
After pressure barreled expires finished product tetrachloro-ethylene, add nitrogen protection.It is placed on warehouse or its fixed-site.
S4 105 DEG C of drying boxes continuous drying two hours, moves into dew by the vial of packing with pure water 3~5 times
Nitrogen purges 30 minutes in -25 DEG C of point glove box below;
Pressurized keg equipped with tetrachloro-ethylene is accessed in glove box with pipeline, dispenses in glove box, keep glove box by S5
- 25 DEG C of dew point or less;
The tetrachloro-ethylene dispensed is added Tetrafluoro spacer, bottle cover for locking, removes glove box, put up label, vacuum plastic sealing by S6.
4. purification, the packing, storage method of a kind of specpure reagent tetrachloro-ethylene according to claim 3, feature exist
In: in step S1, the composite purifying agent is set as natrium carbonicum calcinatum: sodium hydroxide: anhydrous sodium sulfate=1:1:1 mass ratio mixing
Object.
5. purification, the packing, storage method of a kind of specpure reagent tetrachloro-ethylene according to claim 1, feature exist
In: it further include after pressurized keg fills tetrachloro-ethylene finished product, directly moving into warehouse storage, when needing to dispense, with pipeline and gloves
Case connection.
6. purification, the packing, storage method of a kind of specpure reagent tetrachloro-ethylene according to claim 1, feature exist
In: the glove box is purged using preceding with nitrogen, and -25 DEG C of dewpoint requirements or less.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201910287744.9A CN109908617A (en) | 2019-04-11 | 2019-04-11 | A kind of purification of specpure reagent tetrachloro-ethylene, packing, storage method |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201910287744.9A CN109908617A (en) | 2019-04-11 | 2019-04-11 | A kind of purification of specpure reagent tetrachloro-ethylene, packing, storage method |
Publications (1)
Publication Number | Publication Date |
---|---|
CN109908617A true CN109908617A (en) | 2019-06-21 |
Family
ID=66969301
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201910287744.9A Pending CN109908617A (en) | 2019-04-11 | 2019-04-11 | A kind of purification of specpure reagent tetrachloro-ethylene, packing, storage method |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN109908617A (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114392635A (en) * | 2022-02-28 | 2022-04-26 | 稀美资源(广东)有限公司 | Tantalum ethoxide automatic constant-temperature collecting and subpackaging device |
CN115433057A (en) * | 2022-09-08 | 2022-12-06 | 嘉兴学院 | Resourceful treatment method for tetrachloroethylene in fur dry-cleaning waste |
Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1374145A (en) * | 2001-01-17 | 2002-10-16 | Basf公司 | Separation of azeotropic mixture |
CN102690164A (en) * | 2012-06-18 | 2012-09-26 | 贵州威顿晶磷电子材料有限公司 | Method for preparing novel environmental-protection cleaning agent such as electronic grade n-propyl bromide |
CN103209942A (en) * | 2010-11-10 | 2013-07-17 | 中央硝子株式会社 | Process for producing trans-1,3,3,3-tetrafluoropropene |
CN103588615A (en) * | 2013-11-01 | 2014-02-19 | 聊城市鲁西化工工程设计有限责任公司 | Device and technology for recovery of tetrachloroethylene |
JP2016107194A (en) * | 2014-12-04 | 2016-06-20 | 株式会社Stac | Gas recovery system, and gas recovery method |
CN107118074A (en) * | 2017-04-11 | 2017-09-01 | 黎明化工研究设计院有限责任公司 | A kind of method for purifying perfluoromethylcyclohexane (PFMCH) |
CN109369413A (en) * | 2018-10-29 | 2019-02-22 | 邹平铭兴化工有限公司 | The preparation method of diallylamine and its hydrochloride |
CN109456143A (en) * | 2018-11-27 | 2019-03-12 | 郑州师范学院 | The purification process of tetrachloro-ethylene |
-
2019
- 2019-04-11 CN CN201910287744.9A patent/CN109908617A/en active Pending
Patent Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1374145A (en) * | 2001-01-17 | 2002-10-16 | Basf公司 | Separation of azeotropic mixture |
CN103209942A (en) * | 2010-11-10 | 2013-07-17 | 中央硝子株式会社 | Process for producing trans-1,3,3,3-tetrafluoropropene |
CN102690164A (en) * | 2012-06-18 | 2012-09-26 | 贵州威顿晶磷电子材料有限公司 | Method for preparing novel environmental-protection cleaning agent such as electronic grade n-propyl bromide |
CN103588615A (en) * | 2013-11-01 | 2014-02-19 | 聊城市鲁西化工工程设计有限责任公司 | Device and technology for recovery of tetrachloroethylene |
JP2016107194A (en) * | 2014-12-04 | 2016-06-20 | 株式会社Stac | Gas recovery system, and gas recovery method |
CN107118074A (en) * | 2017-04-11 | 2017-09-01 | 黎明化工研究设计院有限责任公司 | A kind of method for purifying perfluoromethylcyclohexane (PFMCH) |
CN109369413A (en) * | 2018-10-29 | 2019-02-22 | 邹平铭兴化工有限公司 | The preparation method of diallylamine and its hydrochloride |
CN109456143A (en) * | 2018-11-27 | 2019-03-12 | 郑州师范学院 | The purification process of tetrachloro-ethylene |
Non-Patent Citations (2)
Title |
---|
国家食品药品监督管理局药品认证管理中心: "《药品GMP指南 无菌药品》", 31 August 2011, 中国医药科技出版社 * |
马世昌: "《化学物质辞典》", 30 April 1999, 陕西科学技术出版社 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114392635A (en) * | 2022-02-28 | 2022-04-26 | 稀美资源(广东)有限公司 | Tantalum ethoxide automatic constant-temperature collecting and subpackaging device |
CN115433057A (en) * | 2022-09-08 | 2022-12-06 | 嘉兴学院 | Resourceful treatment method for tetrachloroethylene in fur dry-cleaning waste |
CN115433057B (en) * | 2022-09-08 | 2023-12-22 | 嘉兴学院 | Method for recycling tetrachloroethylene in fur dry-cleaning waste |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN109908617A (en) | A kind of purification of specpure reagent tetrachloro-ethylene, packing, storage method | |
CN111018662B (en) | Production method for recovering and purifying electronic-grade hexafluoroethane from industrial waste gas generated in carbon tetrafluoride production | |
CN103910333B (en) | A kind of hydrofluoric method in recovery hydrofluorination process tail gas | |
CN1505693A (en) | Use of fluorinated ketones as wet cleaning agents for vapor reactors | |
CN102295521B (en) | Method for preparing tetrachloroethylene through pentachloroethane liquid-phase catalysis | |
US20150108040A1 (en) | Removing mercury from crude oil using a stabilizer column | |
CN101012146A (en) | Method of separating and recovering methyl chloride from methyl chloride mixture gas | |
CN110841453A (en) | Novel high-purity acetylene purification production system and process flow thereof | |
CN101357877B (en) | Method for preparing dibromomethane and methylene chlorobromide by one-pot | |
CN107082407B (en) | A kind of method of purification of anhydrous hydrofluoric acid | |
CN1323992C (en) | Chlorinated tail gas absorbing unit and method for chlorobenzene production | |
Claessens et al. | Capturing renewable isobutanol from model vapor mixtures using an all-silica beta zeolite | |
CN101810982A (en) | Ethanol-containing waste-gas treatment process flow | |
CN100540517C (en) | The method of separating trifluoroethylene during tetrafluoroethylene is produced | |
CN1289448C (en) | Clean reclaiming process for byproduct chloromethane of glyphosate acid | |
CN106621757B (en) | Chlorosilane analysis waste gas recovery treatment device and treatment method | |
CN104768902B (en) | Nitrogen-containing impurity is removed from alcohol composition | |
CN103303894B (en) | Carbonyl fluoride purifying method | |
CN101365669B (en) | Improved fluorination reactor | |
CN214634110U (en) | Hydrochloric acid desorption device using sulfuric acid as extractant | |
CN107008133B (en) | Comprehensive treatment device for waste gas and waste water in benzyl alcohol production | |
CN109847538A (en) | Methylene chloride waste gas processing method | |
CN112473314B (en) | Environment-friendly treatment method for 3-chloropropyl trichlorosilane synthesis tail gas | |
CN206157074U (en) | Novel xylol and recovery of acetic acid waste gas device | |
CN1288118C (en) | Clean reclaiming process for byproduct chloromethane of glyphosate acid |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
CB02 | Change of applicant information | ||
CB02 | Change of applicant information |
Address after: 215500 Xiangqiao village, Zhitang Town, Changshu City, Suzhou City, Jiangsu Province Applicant after: Yonghua Chemical Co.,Ltd. Address before: 215500 Xiangqiao village, Zhitang Town, Changshu City, Suzhou City, Jiangsu Province Applicant before: YONGHUA CHEMICAL TECHNOLOGY (JIANGSU) Co.,Ltd. |
|
RJ01 | Rejection of invention patent application after publication | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190621 |