CN107188995B - A kind of device and its application for adjusting polytetrafluoroethylene (PTFE) reaction temperature - Google Patents
A kind of device and its application for adjusting polytetrafluoroethylene (PTFE) reaction temperature Download PDFInfo
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- CN107188995B CN107188995B CN201610145047.6A CN201610145047A CN107188995B CN 107188995 B CN107188995 B CN 107188995B CN 201610145047 A CN201610145047 A CN 201610145047A CN 107188995 B CN107188995 B CN 107188995B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/01—Processes of polymerisation characterised by special features of the polymerisation apparatus used
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F114/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
- C08F114/18—Monomers containing fluorine
- C08F114/26—Tetrafluoroethene
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- Physical Or Chemical Processes And Apparatus (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention provides a kind of for adjusting the device of polytetrafluoroethylene (PTFE) reaction temperature, including make-up water water inlet pipe, air supply tank, air pressure tank, heating heat exchanger, cooling heat exchanger, ptfe autoclave outer wall collet, make-up water water inlet pipe is connected to air supply tank, the outlet pipeline of air supply tank is connected to air pressure tank, the outlet pipeline of air pressure tank is connected to preheater, the outlet pipeline of preheater is separately connected heating pipeline and cooling line, piping connection heating heat exchanger is heated, heating heat exchanger outlet pipeline connects collet；The heat transferring medium outlet of collet is by piping connection on the outlet pipeline of preheater.The present invention uses deionized water for the temperature control medium in polytetrafluoroethylene (PTFE) reaction process, and deionized water non flouling behaviour in cyclic process improves the precision of temperature control and the quality of polyflon；Entire temperature-adjusting device is closed circulation, does not use industrial water-air cooling cooling, does not have impurity and enters circulation line, temperature control medium loss is few, the advantage with save the cost.
Description
Technical field
The invention belongs to organic high molecular compound preparation fields, and in particular to a kind of emulsion polymerization is temperature controlled
Device and method.
Background technique
Polyflon is widely used because it is with excellent comprehensive performance in current industrial field.Polytetrafluoroethyl-ne
The main production method of alkene is emulsion polymerization, and polymerized monomer is under certain temperature and pressure, in initiator, chain-transferring agent, emulsification
Emulsion polymerization is carried out under agent existence condition.For the polytetrafluoroethyl-ne ene product of different performance, different polymerization temperatures can be used.
In the reaction process of polytetrafluoroethylene (PTFE), the stability of reaction temperature and adjusting sensitivity are to influence end product quality
One highly important factor of height.In current polytetrafluoroethylene (PTFE) industry, the heat exchange of ptfe autoclave uses work
For industry water as tempered water, industry water is impure more, is easy scale effect heat transfer effect, and the adjusting for reducing reaction temperature is sensitive
Degree；It is lost in temperature adjustment water cycle process as tempered water due to directly being contacted with the external world in cooling procedure using industry water
Greatly, production cost is increased.
Summary of the invention
In view of the deficienciess of the prior art, the present invention sets the adjusting technique of polytetrafluoroethylene (PTFE) reaction temperature
Meter, provides a kind of for adjusting the device of polytetrafluoroethylene (PTFE) reaction temperature.
It is another object of the present invention to apply described device, a kind of method for adjusting polytetrafluoroethylene (PTFE) reaction temperature is provided.
Realize the technical solution of above-mentioned purpose of the present invention are as follows:
It is a kind of for adjusting the device of polytetrafluoroethylene (PTFE) reaction temperature, including deionized water adds system and circulating temperature-regulating system
System,
It includes water supply water inlet pipe, air supply tank, air pressure tank that the deionized water, which adds system,；The circulating temperature-regulating system includes
Circulation line, heating heat exchanger, cooling heat exchanger, the collet for being placed in ptfe autoclave outer wall, the collet are provided with
Heat transferring medium import and heat transferring medium outlet；
The make-up water water inlet pipe is connected to the air supply tank, air supply tank outlet pipeline is connected to air pressure tank, air pressure tank
Outlet pipeline is connected with preheater, and the outlet pipeline of preheater is connected to circulating temperature-regulating system；The outlet pipeline of preheater is through following
Endless tube road and three-way control valve are connected separately with heating pipeline and cooling line, heat heat exchange described in the heating piping connection
Device, the heat transferring medium import of the outlet pipeline connection collet of heating heat exchanger；The cooling line connects the cooling heat exchanger,
The heat transferring medium import of the outlet pipeline connection collet of cooling heat exchanger.
Wherein, make-up water water inlet pipe can connect deionized water storage tank, and usual spent ion exchange resin produces deionized water.Folder
The heat transferring medium import of set setting can be 1~4, and the collet of usual bulky reactor can set multiple imports；Collet
The heat transferring medium outlet of setting can be 1~4, and the collet of bulky reactor can set multiple outlets.
Further, the outlet pipeline of the outlet pipeline of the heating heat exchanger and cooling heat exchanger passes through threeway or static state
Mixer links together, the heat transferring medium import of the third outlet connection collet of threeway or static mixer.
Hot water and cold water, which first mix, enters back into collet.Connection water pipe can be threeway or static mixer, when water is big
It is preferred that water preferably uses threeway when few with static mixer.
Wherein, water circulating pump is provided on the circulation line.
Wherein, it is provided with temperature sensor in ptfe autoclave, the heat medium pipeline of the heating heat exchanger,
Valve is provided on the cooling medium pipeline of cooling heat exchanger, the temperature sensor, valve, three-way control valve are all connected to
Automatic control system.
A method of adjusting polytetrafluoroethylene (PTFE) reaction temperature using device of the present invention is poly- with deionized water
Heat transferring medium in tetrafluoroethene reacting kettle jacketing, deionized water are fed from make-up water water inlet pipe, in heating heat exchanger and/or cold
But enter reacting kettle jacketing in heat exchanger after heat exchange, adjust the temperature of polytetrafluoroethyl-ne alkene reaction；Deionized water heat exchange after again into
Enter heating heat exchanger and/or cooling heat exchanger, cycle heat exchange.
Preferably, be 0.2Mpa~0.25Mpa with the pressure of the air supply tank control pressure tank, at the top of air pressure tank from
The liquid level of deionized water is 1/2~2/3 in dynamic exhaust valve Air Valve Control tank.For example, air pressure tank height is 2000mm, then liquid is controlled
Position height is 1000mm~1300mm.
Wherein, temperature is 50 ± 3 DEG C after the deionized water result preheater preheating.The heat medium that preheater uses is
Low-pressure steam (steam of 0.4~1.0Mpa of pressure).
Preferably, the ptfe autoclave volume that the deionized water internal circulating load is 25~35 times per hour.For example,
Reactor volume is 4m3, deionized water internal circulating load is 100~140m3/h。
Wherein, the lift of the water circulating pump is 50m；The range of polytetrafluoroethylene (PTFE) reaction temperature is 73.5~120 DEG C.
Wherein, the heating heat exchanger is plate heat exchanger, and using low-pressure steam as heat medium, the cooling heat exchanger is
Plate heat exchanger, using 4~8 DEG C of water as cooling medium.
The beneficial effects of the present invention are:
The present invention uses deionized water for the temperature control medium in polytetrafluoroethylene (PTFE) production process, and deionized water is in cyclic process
Middle non flouling behaviour improves the precision of temperature control；Entire temperature-adjusting device is closed circulation, does not use industrial water-air cooling cooling,
Impurity is not had and enters circulation line, and temperature control medium loss is few, the advantage with save the cost.
Detailed description of the invention
Fig. 1 is the present invention for adjusting the structure drawing of device of polytetrafluoroethylene (PTFE) reaction temperature.
In figure, 1, reactor, 2, plate type heating heat exchanger, 3, board-like cooling heat exchanger, 4, water circulating pump, 5, air supply tank,
6, air pressure tank, 7, preheater, the 8, first temperature sensor, 9, second temperature sensor, 10, third temperature sensor, 11, automatic
Control system, 12, heat medium valve, 13, cooling medium valve, 14, three-way control valve, 15, regulating valve, 16, check-valves,
17, pressure transmitter, 18, automatic exhaust steam valve, 19, air hose, 20, pre- heat medium pipeline, 21, make-up water water inlet pipe, 22, circulation
Pipeline, 23, the outlet pipeline of preheater
Specific embodiment
Following embodiment further illustrates the contents of the present invention, but should not be construed as limiting the invention.Without departing substantially from
In the case where spirit of that invention and essence, to modifications or substitutions made by the method for the present invention, step or condition, the present invention is belonged to
Range.
Unless otherwise specified, the conventional means that technological means used in embodiment is well known to those skilled in the art.
Embodiment 1
It is a kind of for adjusting the device of polytetrafluoroethylene (PTFE) reaction temperature such as Fig. 1, including deionized water connected from left to right
System and circulating temperature-regulating system are added, is also connected respectively with voltage-stabilizing system and temperature control system；
Specifically, the present apparatus includes make-up water water inlet pipe 21, air pressure tank 6, plate type heating heat exchanger 2, board-like cooling heat transferring
Device 3, be placed in polytetrafluoroethylene (PTFE) polymerization reaction 1 outer wall of reactor collet, which is provided with heat transferring medium import and heat exchange
Media outlet；Regulating valve 15 is set on make-up water water inlet pipe 21.
The make-up water water inlet pipe is connected to the air supply tank 5, the outlet pipeline of air supply tank is connected to air pressure tank 6, air pressure
The outlet pipeline of tank is connected to preheater 7, and the outlet pipeline 23 of preheater connects the circulation line 22 of circulating temperature-regulating system；Circulation
Pipeline 22 is separately connected heating pipeline and cooling line through water circulating pump 4, three-way control valve 14, wherein heating pipeline connecting plate type
Heating heat exchanger 2, the import of the outlet pipeline connection collet of heating heat exchanger；Cooling line connecting plate type cooling heat exchanger 3, it is cold
But the outlet pipeline of the outlet pipeline of heat exchanger and heating heat exchanger is connected by threeway, and the heat transferring medium of collet is entered after merging
Import；The heat transferring medium outlet of collet passes through in piping connection to circulation line 22.The pipeline of the heat transferring medium import connection
Upper setting third temperature sensor 10.
The air pressure tank 6 is connected with air supply tank 5, is provided with non-return on air supply tank top setting air hose 19, air hose 19
Valve 16.Pressure transmitter 17 and automatic exhaust steam valve 18 are set at the top of air pressure tank 6, constitute voltage-stabilizing system.Pressure transmitter 17 connects
The regulating valve 15 of control and recharge water flow excludes more automatically when the liquid level of air pressure tank 6 drops to lower bound, by automatic exhaust steam valve 18
In gas so that its liquid level is maintained at normal within the scope of.In the present embodiment, air pressure tank height 2000mm, the control of intraluminal fluid position
For 1000mm~1300mm.
Water circulating pump 4 is provided on circulation line.The lift of the water circulating pump is 50m.
Wherein, it is provided with two temperature sensors in ptfe autoclave, is the first temperature sensor 8 and respectively
Heat medium valve 12 is arranged on the heat medium pipeline of heating heat exchanger for two temperature sensors 9, the cooling of cooling heat exchanger is situated between
Cooling medium valve 13, the first temperature sensor 8 and second temperature sensor 9, third temperature sensor are provided on matter pipeline
10, heat medium valve 12, cooling medium valve 13, three-way control valve 14 are connected to automatic control system 11.
Embodiment 2
A method of polytetrafluoroethylene (PTFE) reaction temperature being adjusted, the device of embodiment 1 is applied to tetra- fluorine emulsion item of 2500t/a
Purpose production.Using deionized water as the heat transferring medium in ptfe autoclave collet, deionized water spent ion exchange resin
It is prepared, is fed from make-up water water inlet pipe, enter reaction kettle after exchanging heat in heating heat exchanger and/or cooling heat exchanger and press from both sides
Set adjusts the temperature of polytetrafluoroethyl-ne alkene reaction；It is again introduced into heating heat exchanger and/or cooling heat exchanger after deionized water heat exchange,
Cycle heat exchange.
Pressure with the air supply tank control pressure tank is 0.2Mpa~0.25Mpa, with the automatic exhaust at the top of air pressure tank
The liquid level of deionized water is at 1000mm~1300mm height in valve Air Valve Control tank.Air pressure tank height is 2000mm.
In the present embodiment, the tank volume of ptfe autoclave is 4m3, deionized water internal circulating load 120m3/h.Preheating is situated between
It is pre- thermal medium that low-pressure steam is passed through in matter pipeline 20, and deionized water temperature after preheater preheats is 50 ± 3 DEG C.
In the present embodiment, plate type heating heat exchanger is using low-pressure steam as heat medium, and board-like cooling heat exchanger is with 5 DEG C of water
For cooling medium.The range for controlling polytetrafluoroethylene (PTFE) reaction temperature is 73.5~120 DEG C.Temperature fluctuation range exists in production process
Within 1 DEG C.
Temperature control medium is not lost when normal operation；It is using internal cause leakage in 1 year or the waste for overhauling temperature control medium
0.1%
Comparative example
The old tempering process of tetrafluoro resin production project are as follows: the heat transferring medium in the collet of polytetrafluoroethylene (PTFE) polymerization reaction kettle
For industry water.It is divided into two-way from the industry water of the heat transferring medium of collet outlet discharge, is cooling water and non-cooled water respectively, all the way
(cooling water) is reached cooling tower by pipeline and is directly carried out after cooling with non-cooled water using air as cooling medium air-cooled cooling
Enter reactor jacket after mixing to exchange heat.
The tempering process old for polytetrafluoroethyl-ne alkene reaction, the range of temperature adjustment are 73.5~120 DEG C.Temperature in production process
Fluctuation range is within 3 DEG C.
The waste of temperature control medium is 1~2% in 1 year.
Although above the present invention is described in detail with a general description of the specific embodiments,
On the basis of the present invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Cause
This, these modifications or improvements, fall within the scope of the claimed invention without departing from theon the basis of the spirit of the present invention.
Claims (5)
1. a kind of method for adjusting polytetrafluoroethylene (PTFE) reaction temperature, the device of use includes that deionized water adds system and circulation tune
Warm system,
It includes water supply water inlet pipe, air supply tank, air pressure tank that the deionized water, which adds system,；The circulating temperature-regulating system includes circulation
Pipeline, heating heat exchanger, cooling heat exchanger, the collet for being placed in ptfe autoclave outer wall, the collet are provided with heat exchange
Medium entrance and heat transferring medium outlet；
The make-up water water inlet pipe is connected to the air supply tank, air supply tank outlet pipeline is connected to air pressure tank, the water outlet of air pressure tank
Piping connection has preheater, and the outlet pipeline of preheater is connected to circulating temperature-regulating system；The outlet pipeline of preheater is through circulation pipe
Road and three-way control valve are connected separately with heating pipeline and cooling line, and heating heat exchanger described in the heating piping connection adds
The heat transferring medium import of the outlet pipeline connection collet of heat exchanger；The cooling line connects the cooling heat exchanger, cooling
The heat transferring medium import of the outlet pipeline connection collet of heat exchanger；
The method are as follows: using deionized water as the heat transferring medium in ptfe autoclave collet, deionized water is from supply
The supply of water water inlet pipe enters reacting kettle jacketing after exchanging heat in heating heat exchanger and/or cooling heat exchanger, adjusts polytetrafluoroethylene (PTFE)
The temperature of reaction；Heating heat exchanger and/or cooling heat exchanger, cycle heat exchange, with the benefit are again introduced into after deionized water heat exchange
The pressure of gas tank control pressure tank is 0.2Mpa~0.25Mpa, with going in the automatic exhaust steam valve Air Valve Control tank at the top of air pressure tank
The liquid level of ionized water is at 1/2~2/3 height；Deionized water temperature after preheater preheats is 50 ± 3 DEG C, preheater
The heat medium used is low-pressure steam；The ptfe autoclave that the deionized water internal circulating load is 25~35 times per hour
Volume；
The outlet pipeline of the heating heat exchanger and the outlet pipeline of cooling heat exchanger are linked together by threeway, and the of threeway
The heat transferring medium import of three outlet connection collets.
2. adjusting the method for polytetrafluoroethylene (PTFE) reaction temperature according to claim 1, which is characterized in that on the circulation line
It is provided with water circulating pump.
3. adjusting the method for polytetrafluoroethylene (PTFE) reaction temperature according to claim 1, which is characterized in that polytetrafluoroethyl-ne alkene reaction
Temperature sensor is provided on kettle, on the heat medium pipeline of the heating heat exchanger, the cooling medium pipeline of cooling heat exchanger
It is provided with valve, the temperature sensor, valve, three-way control valve are all connected to automatic control system.
4. adjusting the method for polytetrafluoroethylene (PTFE) reaction temperature according to claim 1, which is characterized in that the water circulating pump
Lift is 50m；The range of polytetrafluoroethylene (PTFE) reaction temperature is 73.5~120 DEG C.
5. any method for adjusting polytetrafluoroethylene (PTFE) reaction temperature according to claim 1~4, which is characterized in that described to add
Heat exchanger is plate heat exchanger, and using low-pressure steam as heat medium, the cooling heat exchanger is plate heat exchanger, is with temperature
4~8 DEG C of water is cooling medium.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610145047.6A CN107188995B (en) | 2016-03-14 | 2016-03-14 | A kind of device and its application for adjusting polytetrafluoroethylene (PTFE) reaction temperature |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610145047.6A CN107188995B (en) | 2016-03-14 | 2016-03-14 | A kind of device and its application for adjusting polytetrafluoroethylene (PTFE) reaction temperature |
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| CN107188995B true CN107188995B (en) | 2019-01-04 |
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| CN110005940A (en) * | 2018-01-04 | 2019-07-12 | 中昊晨光化工研究院有限公司 | A kind of tetrafluoroethylene monomer measuring tank and stocking system with air temperature type vaporizer |
| CN112831407A (en) * | 2020-12-25 | 2021-05-25 | 江苏大明生物工程装备有限公司 | Large-scale aerobic fermentation jar with agitator |
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| CN203588092U (en) * | 2013-10-29 | 2014-05-07 | 山东新华医疗器械股份有限公司 | Jacket container temperature control system |
| CN204294227U (en) * | 2014-11-14 | 2015-04-29 | 浙江巨圣氟化学有限公司 | A kind ofly be applied to the polymeric kettle preparing polytetrafluoroethylene (PTFE) |
| CN204544154U (en) * | 2015-03-27 | 2015-08-12 | 诚达药业股份有限公司 | The single heat-conducting medium control device of jacket reactor |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101109966A (en) * | 2007-08-28 | 2008-01-23 | 中昊晨光化工研究院 | Polymer polymerization reaction temperature control method and device thereof |
| CN103588747A (en) * | 2012-08-17 | 2014-02-19 | 中国石油化工股份有限公司 | Production method and apparatus for epsilon-caprolactone |
| CN203588092U (en) * | 2013-10-29 | 2014-05-07 | 山东新华医疗器械股份有限公司 | Jacket container temperature control system |
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