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 PDF

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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
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tetrachloro
ethylene
packing
glove box
purification
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CN201910287744.9A
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Inventor
张路家
顾学峰
戴惠明
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Yonghua Chemical Technology (jiangsu) Co Ltd
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Yonghua Chemical Technology (jiangsu) Co Ltd
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

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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

A kind of purification of specpure reagent tetrachloro-ethylene, packing, storage method
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.
CN201910287744.9A 2019-04-11 2019-04-11 A kind of purification of specpure reagent tetrachloro-ethylene, packing, storage method Pending CN109908617A (en)

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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

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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
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CN115433057B (en) * 2022-09-08 2023-12-22 嘉兴学院 Method for recycling tetrachloroethylene in fur dry-cleaning waste

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