CN209226877U - A kind of purification devices of low boiling point fluid, fluorine-containing compound - Google Patents

A kind of purification devices of low boiling point fluid, fluorine-containing compound Download PDF

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Publication number
CN209226877U
CN209226877U CN201821420323.6U CN201821420323U CN209226877U CN 209226877 U CN209226877 U CN 209226877U CN 201821420323 U CN201821420323 U CN 201821420323U CN 209226877 U CN209226877 U CN 209226877U
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tank
tank body
washing lotion
rectifying column
outlet
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CN201821420323.6U
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张�浩
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Baruch Materials Shenzhen Co ltd
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Bo Rong New Material (shenzhen) Co Ltd
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Abstract

The utility model provides a kind of purification devices of low boiling point fluid, fluorine-containing compound, the tank body one including being provided with inlet and outlet, and having heaters one is arranged in the bottom of the tank body one;The outlet of rectifying column one, the tank body one is connected with the import of rectifying column one;Washing lotion tank;The washing lotion tank top is provided with import, is connected with the outlet of the rectifying column one;Washing lotion tank lower part is provided with drain hole one and drain hole two;PH monitoring device is provided in the middle part of the washing lotion tank;The bottom of the washing lotion tank is provided with external magnetic stirring apparatus;Tank body two, the tank body two are provided with inlet and outlet, and the drain hole two is connected with the import of tank body two, and having heaters two is arranged in the bottom of the tank body two;Rectifying column two, the import of the rectifying column two are connected with the outlet of the tank body two;Product receiving tank, the product receiving tank are connected with the outlet of the rectifying column two, and the bottom of the product receiving tank is provided with low temperature cryostat device.

Description

A kind of purification devices of low boiling point fluid, fluorine-containing compound
Technical field
The utility model belongs to organic scavenging separation technology field more particularly to a kind of low boiling point fluid, fluorine-containing compound Purification devices.
Background technique
The purifying of product and isolation technics are technology component parts crucial in all kinds of chemical industry synthesis techniques, and rectification method is One of the classical way of liquid phase organic matter is purified, there are easy to operate, the advantages such as separating degree height, but for a variety of fluorochemicals But it is not very applicable in.
Different from hydrocarbon, the intermolecular force of fluorochemical is weaker, vaporization identification at different temperatures Degree is not high, also, since fluorochemical synthesis is mostly started with fluorine-containing substrate, and the chemical machine between by-product and principal product Structure, boiling point etc. are often very close, and the boiling point of fluorochemical is often very low, ingredient easy to form between principal product and impurity Complicated azeotropic mixture, cannot achieve with traditional rectificating method and efficiently separates and purify, i.e., the rotation band rectifying imitated using highest Technology is also difficult to realize that one-step method efficiently separates.
Therefore, weak for intermolecular force, how the fluorochemical of low boiling point realizes that efficiently separating for product is pure Change, and reduce loss of product to greatest extent, is one of the key technology for improving fine fluorination work technological level.
Utility model content
The purpose of this utility model is to provide a kind of purification devices of low boiling point fluid, fluorine-containing compound, the utility model In device can effectively improve the purity of fluorochemical.
The utility model provides a kind of purification devices of low boiling point fluid, fluorine-containing compound, including is provided with inlet and outlet Tank body one, having heaters one is arranged in the bottom of the tank body one;
The outlet of rectifying column one, the tank body one is connected with the import of rectifying column one;
Washing lotion tank, the washing lotion tank top are provided with import, are connected with the outlet of the rectifying column one;The washing lotion tank Lower part is provided with drain hole one and drain hole two;PH monitoring device is provided in the middle part of the washing lotion tank;The bottom of the washing lotion tank It is provided with external magnetic stirring apparatus;
Tank body two, the tank body two are provided with inlet and outlet, and the drain hole two is connected with the import of tank body two, institute State the bottom setting having heaters two of tank body two;
Rectifying column two, the import of the rectifying column two are connected with the outlet of the tank body two;
Product receiving tank, the product receiving tank are connected with the outlet of the rectifying column two, the product receiving tank Bottom is provided with low temperature cryostat device.
Preferably, the tank wall thickness of the tank body one is not less than 1cm;
The tank body one is stainless steel tank body;
The set temperature of the heater one is 50~150 DEG C.
Preferably, the number of plates of the rectifying column one is not less than 30;
The reflux ratio of the rectifying column one is 25:1.
Preferably, the drain hole one and drain hole two are distributed in the two sides of the washing lotion tank sustained height.
Preferably, the pH monitoring device includes probe, and the probe gos deep into depth as the 1/ of washing lotion tank diameter 6。
Preferably, the setting speed of the external magnetic means is not less than 600 revs/min.
Preferably, the number of plates of the rectifying column two is not less than 50;The reflux ratio of the rectifying column two is 15:1.
Preferably, the tank body two is stainless cylinder of steel or glass jar;
The set temperature of the heater two is 40~110 DEG C.
Preferably, the volume ratio of the tank body one, washing lotion tank and tank body two is 1:5:1.
Preferably, the set temperature of the low temperature cryostat device is -20 DEG C.
The utility model provides a kind of purification devices of low boiling point fluid, fluorine-containing compound, including is provided with import and goes out Having heaters one is arranged in the bottom of the tank body one of mouth, the tank body one;Rectifying column one, the outlet of the tank body one and rectifying column one Import be connected;Washing lotion tank;The washing lotion tank top is provided with import, is connected with the outlet of the rectifying column one;It is described Washing lotion tank lower part is provided with drain hole one and drain hole two;PH monitoring device is provided in the middle part of the washing lotion tank;The washing lotion tank Bottom be provided with external magnetic stirring apparatus;Tank body two, the tank body two are provided with inlet and outlet, the drain hole two with The import of tank body two is connected, and having heaters two is arranged in the bottom of the tank body two;Rectifying column two, the import of the rectifying column two It is connected with the outlet of the tank body two;Product receiving tank, the product receiving tank are connected with the outlet of the rectifying column two, The bottom of the product receiving tank is provided with low temperature cryostat device.Soda acid between by-product and principal product is utilized in the utility model The difference of property, is aided with two-part rectifier unit, especially suitable for the separation and purifying of all kinds of low boiling point fluid, fluorine-containing compounds, washes Coming into full contact with and purifying for product to be separated and washing lotion is realized using high-speed stirred in flow container, and pH real time monitoring, washing lotion can be at any time Replacement.Device separation accuracy in the utility model is high, and loss of product is small, can operate continuously.
Detailed description of the invention
In order to illustrate the embodiment of the utility model or the technical proposal in the existing technology more clearly, below will be to embodiment Or attached drawing needed to be used in the description of the prior art is briefly described, it should be apparent that, the accompanying drawings in the following description is only It is the embodiments of the present invention, for those of ordinary skill in the art, without creative efforts, also Other attached drawings can be obtained according to the attached drawing of offer.
Fig. 1 is the composition schematic diagram of the utility model purification devices;
Wherein, 1 is tank body one;2 be heater one;3 be rectifying column one;4 be washing lotion tank, and 41 be pH monitoring device, and 42 are Drain hole one, 43 be drain hole two;5 be external magnetic stirring apparatus;6 be tank body two;7 be heater two;8 be rectifying column two;9 For product receiving tank;10 be low temperature cryostat device;11 be sampling pump.
Specific embodiment
The utility model provides a kind of purification devices of low boiling point fluid, fluorine-containing compound, including is provided with import and goes out Having heaters one is arranged in the bottom of the tank body one of mouth, the tank body one;
The outlet of rectifying column one, the tank body one is connected with the import of rectifying column one;
Washing lotion tank;The washing lotion tank top is provided with import, is connected with the outlet of the rectifying column one;The washing lotion tank Lower part is provided with drain hole one and drain hole two;PH monitoring device is provided in the middle part of the washing lotion tank;The bottom of the washing lotion tank It is provided with external magnetic stirring apparatus;
Tank body two, the tank body two are provided with inlet and outlet, and the drain hole two is connected with the import of tank body two, institute State the bottom setting having heaters two of tank body two;
Rectifying column two, the import of the rectifying column two are connected with the outlet of the tank body two;
Product receiving tank, the product receiving tank are connected with the outlet of the rectifying column two, the product receiving tank Bottom is provided with low temperature cryostat device.
In the utility model, for tank body one for holding low boiling point fluid, fluorine-containing compound, low boiling point mentioned here is fluorine-containing Compound refers to that reaction substrate is solid, and product is the compound of low-boiling point liquid after heat resolve, is referred specifically to heat The special perfluoroolefine of the chemical structure of decomposition method production.
The tank body one is provided with inlet and outlet, and the import is connected with sampling pump, for low boiling point is too fluorine-containing Compound is delivered in tank body one;The outlet is connected with the import of rectifying column one, and one bottom of tank body is provided with heating Device one, the heater one are used to heat to the liquid in tank body one, and the set temperature of the heater one is 50~150 DEG C, Preferably 70~120 DEG C, more preferably 80~100 DEG C;Be provided with mechanical stirring device in the tank body one, make pot liquid by It is hot uniform.
The number of plates in the rectifying column one is not less than 30, and reflux ratio is preferably 25:1.
For holding a rectifying product and washing lotion, preferably glass washing lotion tank, thickness is not less than the washing lotion tank 1cm;The washing lotion tank top is provided with import, and the product isolated from rectifying column enters washing lotion by washing lotion tank top entrance Tank;Drain hole one and drain hole two, the drain hole one and drain hole two are provided at the lower part sustained height of the washing lotion tank It is located at the two sides of washing lotion tank, wherein drain hole one is used to release the washing lotion of failure, and drain hole two is for releasing separation product Secondary rectifying is carried out into tank body two.
It is provided with pH monitoring device at the can body 1/2 of the washing lotion tank, for monitoring the pH value of washing lotion pot liquid, if PH value then illustrates that washing lotion fails close to 7, need to stop separating program, the washing lotion of failure is released by drain hole two, and be pumped into new wash Liquid.Washing lotion ingredient can be 10% sodium hydroxide or 15% methylamine or 5% depending on the pH value of impurity in crude product Dilute hydrochloric acid etc..
The pH monitoring device includes by popping one's head in, and the depth that the probe gos deep into washing lotion tank is fill body diameter 1/6.
The bottom of the washing lotion tank is provided with external magnetic stirring apparatus, the setting speed of the external magnetic stirring apparatus Not less than 600 revs/min;High-speed stirred can be realized coming into full contact with and purifying for separation product and washing lotion.
The tank body two can be stainless steel tank body, be also possible to glass tank body, and the tank body two is provided with import and goes out Mouthful, the separation product separated through washing lotion tank enters from the import of tank body two, carries out secondary rectifying;The bottom of the tank body two is arranged Having heaters two, and be provided with mechanical stirring device in tank body two makes heated liquid in tank body two more evenly.
The set temperature of the heater two is 40~110 DEG C, preferably 50~100 DEG C, more preferably 60~80 DEG C.
The number of plates in the rectifying column two is not less than 50, and the reflux ratio of the rectifying column two is preferably 15:1.
The volume ratio of the tank body one, washing lotion tank and tank body two is preferably 1:5:1.
Product through secondary rectifying enters product receiving tank by the outlet of rectifying column two, and the product receives pot bottom and sets It is equipped with low temperature cryostat device, the set temperature of the low temperature cryostat device is -20 DEG C.
It is as follows using the specific purification process of purification devices in the utility model:
Before purifying starts, crude product injects tank body one by sampling pump, and the temperature setting of heater one is 50 degrees Celsius to 150 Between degree Celsius, level-one separation product carries out first time purifying by rectifying column one, flows into washing lotion tank.Washing lotion tank and tank body one Volumetric ratio is 5:1, and the initial reservoir quantity of respective tank body must not be more than the 50% of tank volume.
Magnetic agitation rotating speed in washing lotion tank must not be lower than 600 revs/min, and level-one separation product is instilled by washing lotion tank top Washing lotion tank, is sufficiently mixed with washing lotion under high velocity agitation.Washing lotion ingredient is depending on the impurity pH value in crude product, Ke Yiwei 10% sodium hydroxide, 15% methylamine or 5% dilute hydrochloric acid etc..When reservoir quantity reaches tank volume 80% in washing lotion tank, Heater one stops working, and washing lotion tank continues stirring 20 minutes.Then stop stirring, after stratification, be released by drain hole two Level-one separation product carries out secondary rectifying into tank body two.
Real-time PH monitor is housed, if pH value is close to 7, then washing lotion fails, and need to stop separating program, by blowing in washing lotion tank Mouth one releases failure washing lotion, and is pumped into new washing lotion.
Level-one separation product enters tank body two, and two temperature setting of heater is between 40 degrees Celsius to 110 degrees Celsius.Product After secondary distillation enter product receiving tank, due to the low boiling dot characteristics of final product, receiving tank need to add subzero 20 degrees Celsius it is cold Bath.
The utility model provides a kind of purification devices of low boiling point fluid, fluorine-containing compound, including is provided with import and goes out Having heaters one is arranged in the bottom of the tank body one of mouth, the tank body one;Rectifying column one, the outlet of the tank body one and rectifying column one Outlet be connected;Washing lotion tank;The washing lotion tank top is provided with import, is connected with the outlet of the rectifying column one;It is described Washing lotion tank lower part is provided with drain hole one and drain hole two;PH monitoring device is provided in the middle part of the washing lotion tank;The washing lotion tank Bottom be provided with external magnetic stirring apparatus;Tank body two, the tank body two are provided with inlet and outlet, the drain hole two with The import of tank body two is connected, and having heaters two is arranged in the bottom of the tank body two;Rectifying column two, the import of the rectifying column two It is connected with the outlet of the tank body two;Product receiving tank, the product receiving tank are connected with the outlet of the rectifying column two, The bottom of the product receiving tank is provided with low temperature cryostat device.Soda acid between by-product and principal product is utilized in the utility model The difference of property, is aided with two-part rectifier unit, especially suitable for the separation and purifying of all kinds of low boiling point fluid, fluorine-containing compounds, washes Coming into full contact with and purifying for product to be separated and washing lotion is realized using high-speed stirred in flow container, and pH real time monitoring, washing lotion can be at any time Replacement.Device separation accuracy in the utility model is high, and loss of product is small, can operate continuously.
In order to further illustrate the utility model, with reference to embodiments to a kind of low boiling point liquid provided by the utility model The purification devices of state fluorochemical are described in detail, but cannot be understood as the limit to scope of protection of the utility model It is fixed.
Embodiment 1
Using purification devices shown in FIG. 1, low boiling point perfluoroalkanes compound is purified, process is as follows:
Before purifying starts, crude product (pH is 1 or so) injects tank body one by sampling pump, and the temperature setting of heater one is 70 Between~90 DEG C, level-one separation product carries out first time purifying by rectifying column one, flows into washing lotion tank.Washing lotion tank and tank body one Volumetric ratio is 5:1, and the initial reservoir quantity of respective tank body must not be more than the 50% of tank volume.
Magnetic agitation rotating speed in washing lotion tank must not be lower than 600 revs/min, and level-one separation product is instilled by washing lotion tank top Washing lotion tank, is sufficiently mixed with washing lotion under high velocity agitation.Washing lotion ingredient is 15% methylamine water solution.When reservoir quantity reaches in washing lotion tank When to tank volume 80%, heater one stops working, and washing lotion tank continues stirring 20 minutes.Then stop stirring, stratification Afterwards, level-one separation product is released by drain hole two, carries out secondary rectifying into tank body two.
Real-time pH monitor is housed, if pH value is close to 7, then washing lotion fails, and need to stop separating program, by blowing in washing lotion tank Mouth one releases failure washing lotion, and is pumped into new washing lotion.
Level-one separation product enters tank body two, and two temperature setting of heater is 40~50 DEG C.Product is laggard through secondary distillation Enter product receiving tank, due to the low boiling dot characteristics of final product, receiving tank need to add subzero 20 degrees Celsius of cryostats.Its final product Purity is 98%.
Comparative example 1
Using purification devices shown in FIG. 1, the difference is that, purification devices do not have rectifying column two, tank body two in this comparative example With heater two, drain hole two is directly connected with the import of product receiving tank.
According in embodiment 1 purification process and step to the crude product of low boiling point fluorochemical (pH value is 1 or so) It is purified, the purity of final product is 75%.
Comparative example 2
Using purification devices shown in FIG. 1, the difference is that, purification devices do not have washing lotion tank and external magnetic force in this comparative example The outlet of agitating device, rectifying column one is directly connected with the import of tank body two.
According in embodiment 1 purification process and step to the crude product of low boiling point fluorochemical (pH value is 1 or so) It is purified, the purity of final product is 60%.
The above is only the preferred embodiment of the utility model, it is noted that for the common skill of the art For art personnel, without departing from the principle of this utility model, several improvements and modifications can also be made, these improve and Retouching also should be regarded as the protection scope of the utility model.

Claims (8)

1. a kind of purification devices of low boiling point fluid, fluorine-containing compound, which is characterized in that the tank including being provided with inlet and outlet Having heaters one is arranged in the bottom of body one, the tank body one;
The outlet of rectifying column one, the tank body one is connected with the import of rectifying column one;
Washing lotion tank, the washing lotion tank top are provided with import, are connected with the outlet of the rectifying column one;Washing lotion tank lower part It is provided with drain hole one and drain hole two;PH monitoring device is provided in the middle part of the washing lotion tank;The bottom of the washing lotion tank is arranged There is external magnetic stirring apparatus;
Tank body two, the tank body two are provided with inlet and outlet, and the drain hole two is connected with the import of tank body two, the tank Having heaters two is arranged in the bottom of body two;
Rectifying column two, the import of the rectifying column two are connected with the outlet of the tank body two;
Product receiving tank, the product receiving tank are connected with the outlet of the rectifying column two, the bottom of the product receiving tank It is provided with low temperature cryostat device.
2. purification devices according to claim 1, which is characterized in that the tank wall thickness of the tank body one is not less than 1cm;
The tank body one is stainless steel tank body.
3. purification devices according to claim 1, which is characterized in that the number of plates of the rectifying column one is not less than 30;
The reflux ratio of the rectifying column one is 25:1.
4. purification devices according to claim 1, which is characterized in that the drain hole one and drain hole two are distributed in described The two sides of washing lotion tank sustained height.
5. purification devices according to claim 1, which is characterized in that the pH monitoring device includes probe, the probe Go deep into depth be washing lotion tank diameter 1/6.
6. purification devices according to claim 1, which is characterized in that the number of plates of the rectifying column two is not less than 50;Institute The reflux ratio for stating rectifying column two is 15:1.
7. purification devices according to claim 1, which is characterized in that the tank body two is stainless cylinder of steel or glass jar.
8. purification devices according to claim 1, which is characterized in that the volume of the tank body one, washing lotion tank and tank body two Than for 1:5:1.
CN201821420323.6U 2018-08-30 2018-08-30 A kind of purification devices of low boiling point fluid, fluorine-containing compound Active CN209226877U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201821420323.6U CN209226877U (en) 2018-08-30 2018-08-30 A kind of purification devices of low boiling point fluid, fluorine-containing compound

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201821420323.6U CN209226877U (en) 2018-08-30 2018-08-30 A kind of purification devices of low boiling point fluid, fluorine-containing compound

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Publication Number Publication Date
CN209226877U true CN209226877U (en) 2019-08-09

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GR01 Patent grant
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PE01 Entry into force of the registration of the contract for pledge of patent right

Denomination of utility model: Purification device for low boiling point liquid fluorine-containing compound

Effective date of registration: 20211222

Granted publication date: 20190809

Pledgee: Shanghai Fengfu Investment Co.,Ltd.

Pledgor: BARUCH MATERIALS (SHENZHEN) Co.,Ltd.

Registration number: Y2021310000149

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Date of cancellation: 20220124

Granted publication date: 20190809

Pledgee: Shanghai Fengfu Investment Co.,Ltd.

Pledgor: BARUCH MATERIALS (SHENZHEN) Co.,Ltd.

Registration number: Y2021310000149

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Effective date of registration: 20220314

Address after: 201799 room 2408, Zone C, East podium, building 4, No. 3560, waiqingsong Road, Baihe Town, Qingpu District, Shanghai

Patentee after: Shanghai Fengfu Investment Co.,Ltd.

Address before: 518000 102, building 25, Guangsheng Road, Xin'an street, Bao'an District, Shenzhen City, Guangdong Province

Patentee before: BARUCH MATERIALS (SHENZHEN) Co.,Ltd.

TR01 Transfer of patent right
TR01 Transfer of patent right

Effective date of registration: 20240115

Address after: 518000 102, building 25, Guangsheng Road, Xin'an street, Bao'an District, Shenzhen City, Guangdong Province

Patentee after: BARUCH MATERIALS (SHENZHEN) Co.,Ltd.

Address before: 201799 room 2408, Zone C, East podium, building 4, No. 3560, waiqingsong Road, Baihe Town, Qingpu District, Shanghai

Patentee before: Shanghai Fengfu Investment Co.,Ltd.

TR01 Transfer of patent right