CN104162398B - A kind of annular reactor - Google Patents
A kind of annular reactor Download PDFInfo
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- CN104162398B CN104162398B CN201410399568.5A CN201410399568A CN104162398B CN 104162398 B CN104162398 B CN 104162398B CN 201410399568 A CN201410399568 A CN 201410399568A CN 104162398 B CN104162398 B CN 104162398B
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Abstract
The invention provides a kind of circle shaped tube type reactor, at least include endless tube, charge pump and circulating pump, described endless tube is made up of engineering plastics or the carbon fibre composite of high temperature high voltage resistant, the diameter of endless tube is less than 80mm, on described endless tube, subsection setup has the charging aperture for supplemented by additives, described endless tube is provided with microwave heating system, described microwave heating system includes controller, data wire and the ring shape microwave heater being connected with controller by data wire, described ring shape microwave heaters set is on endless tube, every section of endless tube is all cased with ring shape microwave heater, and the length of this section of endless tube at the length of ring shape microwave heater and its place matches, described controller is provided with control loop, control loop and controlled keying and the watt level of each ring shape microwave heater by data wire. this annular reactor is on the basis of cost of not increasing input, it is possible to each stage of reaction is carried out independent temperature, and temperature is easy to adjust.
Description
Technical field
The invention provides a kind of annular reactor for the polymerization of polymer waterborne emulsion, belong to chemical reaction device technical field.
Background technology
In field of fine chemical, when macromolecular material carries out single liquid phase, liquid liquid phase, gas-liquid equal heterogeneous reaction process, industrial scale produces and adopts tank reactor more, and setting up in reactor has stirring (mechanical agitation, airflow stirring etc.) device. When ratio of height to diameter is bigger, available multiple impellers leaf. In course of reaction, heating material or control that reaction temperature adopts steam to pass into chuck substantially, chuck is inserted into that then electrical bar heats conduction oil, hot water, thermal conductance deep fat heat in modes such as chuck inner-outer circulations, when needing cooling or cooling, then cold water, cold heat conduction wet goods mode is mostly adopted to lower the temperature or cool down. Tank reactor is applied widely, small investment, goes into operation easily, it is possible to changes reaction content easily, is suitable for batch (-type) emulsion polymerization. But course of reaction will experience the process of the computer heating control thermotonus reaction end intensification cooling discharge cleaning reactor that feeds intake every time, adding equipment heat exchange area little, reactor temperature is wayward, and the time of staying of material is also inconsistent, therefore, it is a relatively inefficient use in theory. Even so, prior art carries out the reactor of polymer waterborne emulsion polymerization and almost all adopts tank reactor.
But from polymerization theory, macromolecular material carries out the heterogeneous reaction processes such as single liquid phase, liquid liquid phase, liquid phase and pressurization, desirably displacement flow reactor should be the tubular reactor of annular. This reactor volume is less, and the heat transfer area of unit volume is big, and safety is high. During polyreaction, the molecule of reactant time of staying in reactor is equal, the reactant concentration on any point and chemical reaction velocity not times to time change in reactor, only change with pipe range, during polymerization, response speed is fast, flow velocity speed is adjustable, can pass through during operation to control reaction time, reaction temperature and pressure, realize limit charging, limit go out finished product continuous polymerization reaction, production capacity is high, is particularly well-suited to the bigger polyreaction of heat effect and the emulsion polymerization of maximization, serialization.Regrettably, although the annular reactor of prior art speak from polymerization theory be a kind of desirable polymer waterborne emulsion polymerization equipment, but reflect in production practices and application practice some problems always fail solve.
For ethylene-vinyl acetate emulsion (VAE emulsion) polyreaction, its process carrying out polymerization technique at high pressure annular reactor is: be first dissolved in water by PVA, reducing agent, buffer agent etc., make aqueous phase, then pass through plunger displacement pump and be continuously injected in endless tube, ON cycle pump is also injected separately into monomer phase and initiator, now reaction temperature can be increased to setting value automatically, realizes automatically controlling of temperature by recirculating cooling water system. Pass into the ethylene of setting again, and by the pressure of the standby pressure valve adjustment endless tube of outlet to analog value (being generally 4��9mPa), after ethylene passes into 0.5h, stability index is reached from endless tube discharging opening material out, namely it is transported in another container, carry out the post processing of residual monomer or add the programs such as auxiliary agent, filtration, discharging, packaging after qualified. From whole technical process, various materials constant speed always adds, and reacts stable homogeneous, and whole polymerization process is ideal, but, the investment of segmentation analysis annular reactor, feed intake, produce, the overall process of finished product application, it has been found that there are problems:
One. product emulsion quality problems
When the detection of emulsion manufactured goods every physical index is all qualified, the product that the VAE emulsion that annular reactor produces produces with autoclave when practical application is adopted to contrast, there is solvent thickening not notable, the problem that water viscosity just sharply declines a little, such VAE emulsion often cannot be modified processing by this;
Even if every physical characteristic detects the factory calibration meeting VAE emulsion but every application indexes can not compare favourably with the VAE emulsion that autoclave produces completely.
For the problems referred to above, annular reactor is found compared with the course of reaction of step tank reactor, polymer waterborne emulsion polyreaction in batch (-type) tank reactor needs experienced three stages, stage I (nucleation and emulsion particle generation phase): start to micelle all to disappear from being polymerized, along with being continuously increased of emulsion particle number, polymerization rate is incremented by; Stage II (emulsion particle generation phase): disappear starting to disappear to monomer droplet from micelle, this stage emulsion particle number keeps constant, monomer droplet constantly provides monomer to maintain stablizing of monomer concentration to emulsion particle, and rate of polymerization is held essentially constant; Stage III (polymerization deceleration polyreaction completes the stage): disappear to polymerization from monomer droplet and terminate; In the actual control of polyreaction, three above different phase is progressively polymerized in batch (-type) tank reactor, the requirement of temperature is that different (many reactors are not because use adjustable speed to stir by each stage, and what adopt is the mode of automatic flow meter control flow when dripping material), therefore temperature controls the actual most important means becoming and controlling batch (-type) tank reactor reactive state.
Review the annular reactor polymerization process of prior art, various materials always are that constant speed adds, therefore the molecule of polymerization reactant time of staying in reactor is equal, the reactant concentration on any point and chemical reaction velocity in reactor, reaction temperature does not change with the response time, only change with the temperature of recirculated water, react also stable homogeneous, the height of the temperature of recirculated water almost determines reactive state and the result of tubular type emulsion polymerization process, under such reaction condition, the formation of polyalcohol emulsion particle, it is practically without the three phases of experience batch (-type) tank reactor, therefore the latex particle size of annular reactor wider distribution compared with the latex particle size of step tank reactor, solvent is difficult to thickening, the problem that the viscosity that adds water sharply declines and latex particle size wider distribution have very big relation.
Two. the inconspicuous problem of superiority of effectiveness of equipment investment
From annular reactor overall process, reaction terminates rear discharging opening material out and also needs to be transported to another with in chuck, liftable temperature, tank vessel with agitator, just can carry out the post processing of residual monomer and add additive mixture;
Annular reactor is to the gradient of temperature controlling in endless tube and to process residual monomer by cold and hot adjustable deionized water, and jacket type tank vessel requires over hot water or steam provides thermal source, therefore, boiler and deionized water heating and temperature cycles adjustment system also must be equipped with simultaneously;
Seen by above analysis, the birth of annular reactor is because small volume, the heat transfer area of unit volume is big, safety is high, and especially easy realize produce automatization, scale, serialization, should have small investment, the advantage that floor space is little, owing to needing to increase by one with chuck, liftable temperature, carry out post processing with the tank vessel of agitator is supporting, also separately needing boiler and deionized water heating and temperature cycles to regulate system support, therefore the superiority of effectiveness of equipment investment is inconspicuous;
The two class problems reflected in application practice produced above, result in annular reactor and rarely have application in production practices.
The current market competition is more and more fierce, the annular reactor limit charging of prior art, limit go out the continuous prodution mode of finished product, it is particularly suitable for the automation size production that all computer controls, therefore, solve the problem restricting its application that the annular reactor of prior art exists, be the hope of business circles and scientific and technological circle.
Summary of the invention
The invention provides a kind of annular reactor, solve the deficiency in background technology, this annular reactor is on the basis of cost of not increasing input, it is possible to each stage of reaction is carried out independent temperature, and temperature is easy to adjust.
Realizing the technical scheme that above-mentioned purpose of the present invention adopts is:
A kind of circle shaped tube type reactor, at least include endless tube, charge pump and circulating pump, described endless tube is made up of engineering plastics or the carbon fibre composite of high temperature high voltage resistant, the diameter of endless tube is less than 80mm, on described endless tube, subsection setup has the charging aperture for supplemented by additives, described endless tube is provided with microwave heating system, described microwave heating system includes controller, data wire and the ring shape microwave heater being connected with controller by data wire, described ring shape microwave heaters set is on endless tube, every section of endless tube is all cased with ring shape microwave heater, and the length of this section of endless tube at the length of ring shape microwave heater and its place matches, described controller is provided with control loop, control loop and controlled keying and the watt level of each ring shape microwave heater by data wire.
Annular reactor provided by the present invention compared with prior art has the advantage that in the application, the material of endless tube is engineering plastics or the carbon fiber of high temperature high voltage resistant, but not metal rustless steel used in the prior art, on each section of endless tube, equal correspondence is provided with ring shape microwave heater, what therefore ring shape microwave heater can be independent is heated each section of endless tube, and heat time heating time and heating power can be controlled by controller, regulate. Circulation hot water or cold water's heating with existing annular reactor is compared with the mode controlling the interior temperature of pipe, the ring shape microwave heater radiated microwaves that the application adopts produces heat to be had selection and high directivity and can inside and outside run through the feature of heating aqueous phase liquid simultaneously, there is no conduction of heat inertia after microwave heating simultaneously, this feature both can save the electric energy of 40��60%, and is easier to control and operation. Meanwhile, in the present invention, when the length of endless tube is inadequate, can suitably increase endless tube length, can two, three endless tube series connection use when condition is restricted.The each section of charging aperture being provided with on endless tube can add various additives according to the obstructed stage of reaction, such as initiator, emulsifying agent, molecular weight regulator etc.
Accompanying drawing explanation
Fig. 1 is the structural representation of annular reactor provided by the invention;
In figure: 1-endless tube, 2-charging aperture, 3-ring shape microwave heater, 4-data wire, 5-controller.
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention done detailed specific description, but protection scope of the present invention is not limited to following example.
The structure of annular reactor provided by the invention is as it is shown in figure 1, at least include endless tube 1, charge pump and circulating pump, and in Fig. 1, charge pump and circulating pump do not show.
Described endless tube 1 is made up of engineering plastics or the carbon fibre composite of high temperature high voltage resistant, and the diameter of endless tube 1 is less than 80mm, and on described endless tube 1, subsection setup has the charging aperture 2 for supplemented by additives.
Described endless tube 1 is provided with microwave heating system, described microwave heating system includes controller 5, data wire 4 and the ring shape microwave heater 3 being connected by data wire 4 with controller 5, described ring shape microwave heater 3 is enclosed within endless tube 1, every section of endless tube 1 is all cased with ring shape microwave heater 3, and the length of this section of endless tube 1 at the length of ring shape microwave heater 3 and its place matches, described controller 5 is provided with control loop, controls loop and controlled keying and the watt level of each ring shape microwave heater by data wire.
Claims (1)
1. the polymer waterborne emulsion polymerization technique based on annular reactor, described annular reactor at least includes endless tube, charge pump and circulating pump, described endless tube is made up of engineering plastics or the carbon fibre composite of high temperature high voltage resistant, the diameter of endless tube is less than 80mm, on described endless tube, subsection setup has the charging aperture for supplemented by additives, described endless tube is provided with microwave heating system, described microwave heating system includes controller, data wire and the ring shape microwave heater being connected with controller by data wire, described ring shape microwave heaters set is on endless tube, every section of endless tube is all cased with ring shape microwave heater, and the length of this section of endless tube at the length of ring shape microwave heater and its place matches, described controller is provided with control loop, control loop and controlled keying and the watt level of each ring shape microwave heater by data wire,
It is characterized in that, ring shape microwave heater independence each section of endless tube is heated, heat time heating time and heating power can be controlled by controller, regulates so that polyreaction experiences the following three stage: (1), start to micelle all to disappear from polymerization; (2), start to monomer droplet to disappear from micelle disappearance; (3), disappear to polymerization from monomer droplet and terminate;
Carrying out in each section in endless tube successively of each stage above, each section of charging aperture being provided with on endless tube can add various additives according to the different stages of reaction.
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| CN201410399568.5A CN104162398B (en) | 2014-08-14 | 2014-08-14 | A kind of annular reactor |
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| CN201410399568.5A CN104162398B (en) | 2014-08-14 | 2014-08-14 | A kind of annular reactor |
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| CN104162398B true CN104162398B (en) | 2016-06-08 |
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| CN112705150B (en) * | 2020-11-05 | 2022-12-23 | 中国恩菲工程技术有限公司 | Composite material preparation device and method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010207735A (en) * | 2009-03-10 | 2010-09-24 | National Institute Of Advanced Industrial Science & Technology | Microwave continuous irradiation method and apparatus to fluid |
| CN102964017A (en) * | 2012-06-07 | 2013-03-13 | 刘风鸣 | Method for treatment of high salinity organic wastewater through microwave electrocatalytic oxidation |
| US20130253089A1 (en) * | 2012-03-09 | 2013-09-26 | Basf Se | Continuous process for the synthesis of graft polymers based on polyethers |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EA200601490A1 (en) * | 2004-02-13 | 2007-02-27 | Тотал Петрокемикалс Рисерч Фелюй | MULTI-CONTOUR REACTOR FOR POLYMERIZATION OF OLEFINS |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010207735A (en) * | 2009-03-10 | 2010-09-24 | National Institute Of Advanced Industrial Science & Technology | Microwave continuous irradiation method and apparatus to fluid |
| US20130253089A1 (en) * | 2012-03-09 | 2013-09-26 | Basf Se | Continuous process for the synthesis of graft polymers based on polyethers |
| CN102964017A (en) * | 2012-06-07 | 2013-03-13 | 刘风鸣 | Method for treatment of high salinity organic wastewater through microwave electrocatalytic oxidation |
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Address after: 430011 Hubei province Wuhan City Jiang'an District Han Huang Road No. 888 B District No. 1 Patentee after: Wuhan hold Technology Co., Ltd. Address before: 430011 Hubei province Wuhan City Jiang''an District Han Huang Road No. 888 B District No. 1 Patentee before: WUHAN JIE FENG JOINT ADHESIVE TECHNOLOGY CO., LTD. |
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Effective date of registration: 20191101 Address after: 226300 No.2, sunliqiao Industrial Park, Xingdong street, Tongzhou District, Nantong City, Jiangsu Province Patentee after: Nantong Braun refrigeration equipment Co., Ltd. Address before: 430011, building 1, B District, 888 Huang Han Road, Jiang'an District, Wuhan, Hubei Patentee before: Wuhan hold Technology Co., Ltd. |