CN110732298A - Microwave radiation continuous water-based resin synthesis pipeline reactor - Google Patents

Microwave radiation continuous water-based resin synthesis pipeline reactor Download PDF

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Publication number
CN110732298A
CN110732298A CN201911146161.0A CN201911146161A CN110732298A CN 110732298 A CN110732298 A CN 110732298A CN 201911146161 A CN201911146161 A CN 201911146161A CN 110732298 A CN110732298 A CN 110732298A
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temperature bath
constant temperature
pumps
tubes
inlets
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CN201911146161.0A
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CN110732298B (en
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张善志
陈华法
徐卡特
徐群策
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WENZHOU GUOSHIBANG POLYMER MATERIALS CO Ltd
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WENZHOU GUOSHIBANG POLYMER MATERIALS CO Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/12Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
    • B01J19/122Incoherent waves
    • B01J19/126Microwaves
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24Stationary reactors without moving elements inside
    • B01J19/2415Tubular reactors

Abstract

The invention relates to an microwave radiation continuous water-based resin synthesis pipeline reactor which is characterized by comprising a left constant temperature bath and a right constant temperature bath which are arranged in parallel, a plurality of groups of serial capillary tubes, multi-channel peristaltic pumps, single-channel peristaltic pumps, a plurality of microwave generators, two cross micro mixers, emulsification pumps, a centrifugal pump and a second centrifugal pump, wherein a plurality of groups of serial capillary tubes, a plurality of microwave generators and temperature detectors are arranged in the inner cavities of the left constant temperature bath and the right constant temperature bath, and the capillary tubes form the continuous pipeline reactor.

Description

Microwave radiation continuous water-based resin synthesis pipeline reactor
Technical Field
The invention relates to a water-based resin synthesis pipeline reaction device, which is suitable for a manufacturing process device of water-based polyurethane dispersion resin.
Background
The existing reaction device for the aqueous polyurethane dispersion resin, , is a batch type kettle reactor or a semi-continuous cavity reactor, and cannot form a continuous reaction device.
However, the intermittent reaction device requires a large manufacturing space, and a large amount of materials require a large-capacity pump, a large-capacity pipeline and a large-capacity reaction kettle to perform daily production work, so that the device is high in danger; and the intermittent reaction device can not ensure the continuous production of the product. The traditional manufacturing mode reaches the bottleneck of industrial preparation technology, the equipment cost is high, and the maintenance cost is also high.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a microwave radiation continuous type water-based resin synthesis pipeline reactor for water-based resins, which has the advantages of good synthesis effect, high efficiency, good safety of production process and low equipment cost and maintenance cost.
The invention relates to a microwave radiation continuous type water-based resin synthesis pipeline reactor which is characterized by comprising a left constant temperature bath and a right constant temperature bath which are arranged in parallel, a plurality of groups of serial capillary tubes, multi-channel peristaltic pumps, single-channel peristaltic pumps, a plurality of microwave generators, two cross micro mixers, emulsification pumps, a centrifugal pump and a second centrifugal pump, wherein the left constant temperature bath and the right constant temperature bath are made of stainless steel materials, inner cavities of the left constant temperature bath and the right constant temperature bath are mutually communicated, the inner cavities of the left constant temperature bath and the right constant temperature bath are provided with a plurality of groups of serial capillary tubes, a plurality of microwave generators and temperature detectors, capillary tube inlets of the left upper inner cavities of the left constant temperature bath and the right constant temperature bath are respectively provided with cross micro mixers, medium circulation outlets are arranged at capillary tube outlets of the right upper inner cavities of the left constant temperature bath and the right constant temperature bath, a medium circulation inlet is arranged at the left lower part of the left constant temperature bath, a medium circulation inlet of the left constant temperature bath is communicated with a medium circulation outlet through a , a medium circulation inlet of the left constant temperature bath is communicated with a medium circulation outlet of the right constant temperature bath, a multi-channel peristaltic pump is communicated with a high-temperature emulsion solution tank through a high-phase emulsion solution mixing tank, a high-phase emulsion solution tank is communicated with a high-phase emulsion solution high-phase emulsion-phase high-phase emulsion-phase high-phase.
In the technical scheme, the capillary tubes are polytetrafluoroethylene tubes with the inner diameter of 0.2-2.0mm, 5-10 capillary tubes are arranged in a tube array type and are tied up by a polytetrafluoroethylene binding tape, and each tube array is arranged in the left constant temperature bath tank and the right constant temperature bath tank side by side.
In the technical scheme, the cross micro mixer is made of stainless steel materials and is provided with a plurality of spigots, and the volume of an inner cavity of the cross micro mixer is 0.2-2.0 ml.
In the technical scheme, the multi-channel peristaltic pump is at least provided with three channels, and the flow rate of the multi-channel peristaltic pump is 10-50 ml/min; the flow rate of the single-channel peristaltic pump is 0.2-10 ml/min.
Compared with the prior art, the invention has the beneficial effects that: a continuous pipeline reactor is formed by adopting capillary tubes, the heat effect of microwave radiation polar medium is used as a heat source, and the reaction speed of reaction substances in the capillary tubes is improved by utilizing microwave radiation. The method has the advantages of good resin synthesis effect, high efficiency, good safety of the production process, low equipment cost and maintenance cost and the like.
Drawings
Fig. 1 is a schematic structural view of the present invention.
In the figure, 1, a polyol solution overhead tank, 2, an isocyanate solution overhead tank, 3, a chain extender, a solvent and catalyst solution overhead tank, 4, a chain extender solution overhead tank, 5, a deionized water overhead tank, 6, a multi-channel peristaltic pump, 7, a cross micro mixer, 8, a microwave generator, 9, a temperature detector, 10, a medium outlet, 11, a single-channel peristaltic pump, 12, a capillary array tube, 13, an emulsification pump, 14, an emulsion storage tank, 15, a th centrifugal pump, 16 a left constant temperature bath, 17, a medium inlet, 18, a right constant temperature bath, 19 and a second centrifugal pump.
Detailed Description
The microwave radiation continuous type water-based resin synthesis pipeline reactor shown in figure 1 is characterized by comprising a left constant temperature bath 16 and a right constant temperature bath 18 which are arranged in parallel, a plurality of groups of serial capillary tubes 12, multi-channel peristaltic pumps 6, single-channel peristaltic pumps 11, a plurality of microwave generators 8, two cross micro mixers 7, emulsion pumps 13, a centrifugal pump 15 and a second centrifugal pump 19, wherein the left constant temperature bath 16 and the right constant temperature bath 18 are made of stainless steel materials, the inner cavities are communicated with each other, a plurality of groups of serial capillary tubes 12, a plurality of microwave generators 8 and temperature detectors 9 are respectively arranged in the inner cavities of the left constant temperature bath 16 and the right constant temperature bath 18, cross micro mixers are respectively arranged at the inlets of the capillary tubes 12 in the inner cavities at the upper left upper parts of the left constant temperature bath 16 and the right constant temperature bath 18, medium circulation outlets are arranged at the outlets of the capillary tubes 12 in the inner cavities at the left constant temperature bath 16 and the right constant temperature bath 18 upper parts of the left constant temperature bath 16 and the right constant temperature bath 18, medium circulation inlets are respectively communicated with the inner cavities of the right constant temperature bath 18 through a high temperature peristaltic pumps 14, a high temperature pump 16, a high temperature pump 13, a medium circulation tank 14 is arranged in the left constant temperature bath 6, a high temperature pump 7, a high temperature pump 13, a high temperature pump 7 is communicated with a high temperature pump 13, a high temperature pump 14, a high temperature pump 13, a high temperature pump 7 is arranged in the high temperature pump, a high temperature pump 13, a high temperature pump 7 is communicated with a high temperature pump 14.
The capillary tubes 12 are formed by arranging 5-10 capillary tubes in a tube array type and fastening the capillary tubes through polytetrafluoroethylene ribbons, each tube array is arranged in a left constant temperature bath groove 16 and a right constant temperature bath groove 18 in parallel, the capillary tubes are polytetrafluoroethylene tubes, the inner diameter of each capillary tube is 0.2-2.0mm, adjacent capillary tubes 12 are connected in series, and the capillary tubes in rows of capillary tubes 12 are connected in series.
The cross micro mixer 7 is made of stainless steel material and is provided with a plurality of spigots, and the volume of the inner cavity of the cross micro mixer is 0.2-2.0 ml. The cross micro mixer 7 is fixedly arranged on a constant left temperature bath groove 16 and a right temperature bath groove 18.
The multi-channel peristaltic pump 6 is at least three channels, and the flow rate is 10-50 ml/min; the flow rate of the single-channel peristaltic pump 11 is 0.2-10 ml/min.
The working process of the invention is as follows:
placing the prepared raw material solution in a polyol solution overhead tank 1, an isocyanate solution overhead tank 2, a chain extender, a solvent and catalyst solution overhead tank 3, a chain extender solution overhead tank 4 and a deionized water overhead tank 5, setting flow parameters of a multi-channel peristaltic pump 6 and a single-channel peristaltic pump 11 according to the proportion, firstly opening an centrifugal pump 15 and a second centrifugal pump 19, starting a microwave generator 8 and a temperature detector 9, heating to a preset temperature and maintaining the temperature at +/-2 DEG C0C; starting a multi-channel peristaltic pump 6, conveying prepolymer reaction materials into a left constant-temperature bath 16, and reacting for 1-3 hours at a set temperature; when the preset time is reached, starting the single-channel peristaltic pump 11, conveying the materials in the chain extender solution head tank 4 into the right constant temperature bath tank 18 for chain extension reaction, and reacting for 1-3 hours at the preset temperature; the materials are output to an emulsification pump 13 through a capillary tube, emulsified into dispersion or emulsion through deionized water, and overflowed to an emulsion storage tank 14.
In the reaction process, the flow rate of the materials in the capillary tube 12 in the left constant temperature bath 16 is 0.5-2.0 m/s; the flow rate of the materials in the capillary tube 12 in the right constant temperature bath 18 is 0.5-2.0 m/s; the material is first mixed initially by means of a cross micro mixer 7 and then thoroughly mixed by the rapid flow in the capillary array 12 and the bend and wall formed by the capillary array 12. The material retention time in the left constant temperature bath 16 and the right constant temperature bath 18 is about 1-3 hours, and the internal material is about 2.0-5.0L. The continuous pipeline reactor can prepare 12-18L products in one day and 4000-6000L products in one year, and has high production efficiency. In the whole process flow, the solution is sealed in the left constant temperature bath 16 and the right constant temperature bath 18 for reaction, and the solution does not contact with the outside air, so that the production safety is good.
The reaction temperature in the left constant temperature bath 16 and the right constant temperature bath 18 is determined by the boiling point of the medium, the reaction temperature of the -shaped prepolymer is 70-90 ℃, and the reaction temperature of the chain extension is 50-80 ℃.
The material in the capillary tubes 12 is affected by microwave radiation, and due to the characteristics of the microwave radiation, the effective distance from the microwave generator is within 25cm, and the chemical reaction of polar molecules is accelerated. And the left and right constant temperature baths 16 and 18 are made of stainless steel and sealed to shield the operator from microwaves.
The continuous pipe reactor of the present invention can be applied to special monomer synthesis and other chemical reactions by changing part of reaction parameters.
The continuous pipeline reactor is reactors capable of continuously operating, and can continuously operate for months or years under the condition of ensuring full supply of materials and normal operation of equipment.

Claims (5)

  1. The microwave radiation continuous type water-based resin synthesis pipeline reactor is characterized by comprising a left constant temperature bath (16) and a right constant temperature bath (18) which are arranged in parallel, a plurality of groups of serial capillary column tubes (12), multi-channel peristaltic pumps (6), single-channel peristaltic pumps (11), a plurality of microwave generators (8), two cross micro mixers (7), emulsion pumps (13), a centrifugal pump (15) and a second centrifugal pump (19), wherein the left constant temperature bath (16) and the right constant temperature bath (18) are made of stainless steel materials and are communicated with each other, a plurality of groups of serial capillary column tubes (12) and a plurality of microwave generators (8) are respectively arranged in inner cavities of the left constant temperature bath (16) and the right constant temperature bath (18), temperature detectors (9) are respectively arranged in the left constant temperature bath (16) and the right constant temperature bath (18), inlets of the capillary column tubes (12) in the left upper inner cavities of the left constant temperature bath (16) and the right constant temperature bath (18) are respectively provided with cross micro mixers, inlets of the cross micro mixers are respectively arranged in inlets of the capillary column tubes (12) in the left constant temperature bath (16) and the right constant temperature bath (18), the inner cavities of the constant temperature bath (18), the emulsion pumps are respectively communicated with inlets of the cross micro solution pumps (13), the cross micro solution mixers in the left constant temperature bath tanks (6), the left constant temperature bath (6) through inlets and right chain pumps, the inlets of the cross micro solution pumps, the cross micro solution pumps (6) and the inlets of the cross micro solution pumps, the cross micro solution mixers, the cross emulsion pumps (6) are respectively communicated with outlets of the cross emulsion pumps (13), the cross emulsion pumps (10) through inlets of the high temperature pumps, the high temperature bath inlets of the high temperature bath (6), the high temperature bath (13), the high temperature bath (18), the high temperature pumps (13.
  2. 2. The continuous microwave radiation type water-based resin synthesis pipeline reactor as claimed in claim 1, wherein the capillary array tubes (12) are arranged in a row tube manner by every 5-10 capillary tubes and are fastened by a polytetrafluoroethylene binding tape, each row tube is arranged in the constant left temperature bath (16) and the constant right temperature bath (18) side by side, the capillary tubes are polytetrafluoroethylene tubes, the inner diameter of each capillary tube is 0.2-2.0mm, adjacent capillary array tubes (12) are connected in series, and the capillary tubes in rows of capillary array tubes (12) are connected in series.
  3. 3. The continuous microwave radiation aqueous resin synthesis pipe reactor as claimed in claim 1 or 2, wherein: the cross micro mixer (7) is made of stainless steel material and is provided with a plurality of spigots, and the volume of the inner cavity of the cross micro mixer is 0.2-2.0 ml.
  4. 4. The continuous microwave radiation aqueous resin synthesis pipe reactor as claimed in claim 1 or 2, wherein: the multi-channel peristaltic pump (6) is at least three channels, and the flow rate is 10-50 ml/min; the flow rate of the single-channel peristaltic pump (11) is 0.2-10 ml/min.
  5. 5. The continuous microwave radiation aqueous resin synthesis pipe reactor as claimed in claim 3, wherein: the multi-channel peristaltic pump (6) is at least three channels, and the flow rate is 10-50 ml/min; the flow rate of the single-channel peristaltic pump (11) is 0.2-10 ml/min.
CN201911146161.0A 2019-11-21 2019-11-21 Microwave radiation continuous water resin synthesis pipeline reactor Active CN110732298B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112354198A (en) * 2020-09-14 2021-02-12 温州国仕邦高分子材料有限公司 Continuous acetone evaporator

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CN101058734A (en) * 2007-05-31 2007-10-24 张付舜 Device for industrially synthesizing biological diesel oil by microwave and method thereof
US20080096118A1 (en) * 2006-10-19 2008-04-24 Fuji Xerox Co., Ltd. Polyester resin and manufacturing method thereof, electrostatic-image-developing toner, developing apparatus, cartridge, image-forming apparatus, and micro-reactor apparatus
CN101450300A (en) * 2007-12-05 2009-06-10 海南大学 Continuous current micro-reactor and preparation method and use thereof
US20100216964A1 (en) * 2005-11-23 2010-08-26 Hte Aktiengesellschaft The High Throughput Experimentation Company Method for producing aryl-aryl coupled compounds
WO2011019184A2 (en) * 2009-08-10 2011-02-17 엔바로테크 주식회사 Method and apparatus for producing a nanoscale material having a graphene structure
CN106925195A (en) * 2015-12-31 2017-07-07 中国石油天然气股份有限公司 A kind of hydro-thermal method prepares the device of powder body material
CN107033030A (en) * 2017-05-10 2017-08-11 大连微凯化学有限公司 A kind of production technology of continuous aniline-acetonitrile
CN211246513U (en) * 2019-11-21 2020-08-14 温州国仕邦高分子材料有限公司 Microwave radiation continuous water-based resin synthesis pipeline reactor

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100216964A1 (en) * 2005-11-23 2010-08-26 Hte Aktiengesellschaft The High Throughput Experimentation Company Method for producing aryl-aryl coupled compounds
US20080096118A1 (en) * 2006-10-19 2008-04-24 Fuji Xerox Co., Ltd. Polyester resin and manufacturing method thereof, electrostatic-image-developing toner, developing apparatus, cartridge, image-forming apparatus, and micro-reactor apparatus
CN101058734A (en) * 2007-05-31 2007-10-24 张付舜 Device for industrially synthesizing biological diesel oil by microwave and method thereof
CN101450300A (en) * 2007-12-05 2009-06-10 海南大学 Continuous current micro-reactor and preparation method and use thereof
WO2011019184A2 (en) * 2009-08-10 2011-02-17 엔바로테크 주식회사 Method and apparatus for producing a nanoscale material having a graphene structure
CN106925195A (en) * 2015-12-31 2017-07-07 中国石油天然气股份有限公司 A kind of hydro-thermal method prepares the device of powder body material
CN107033030A (en) * 2017-05-10 2017-08-11 大连微凯化学有限公司 A kind of production technology of continuous aniline-acetonitrile
CN211246513U (en) * 2019-11-21 2020-08-14 温州国仕邦高分子材料有限公司 Microwave radiation continuous water-based resin synthesis pipeline reactor

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112354198A (en) * 2020-09-14 2021-02-12 温州国仕邦高分子材料有限公司 Continuous acetone evaporator

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