CN105566527A - Reaction device and technology for preparing chlorosulfonated chloroethylene through gas-solid phase method - Google Patents
Reaction device and technology for preparing chlorosulfonated chloroethylene through gas-solid phase method Download PDFInfo
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- CN105566527A CN105566527A CN201610075569.3A CN201610075569A CN105566527A CN 105566527 A CN105566527 A CN 105566527A CN 201610075569 A CN201610075569 A CN 201610075569A CN 105566527 A CN105566527 A CN 105566527A
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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
- C08F8/00—Chemical modification by after-treatment
- C08F8/34—Introducing sulfur atoms or sulfur-containing groups
- C08F8/38—Sulfohalogenation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/1809—Controlling processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/24—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00017—Controlling the temperature
- B01J2208/00026—Controlling or regulating the heat exchange system
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- Combustion & Propulsion (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
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- Polymers & Plastics (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A reaction device and technology for preparing chlorosulfonated chloroethylene through a gas-solid phase method are used for synthesis and production of high-polymer chlorosulfonated polyethylene. Gas-solid phase materials are adopted for performing an incurring and initial reaction in a lifting pipe in the circulating process, a deep reaction is performed in a fluidized bed reactor, the incurring strength and the reaction process are controlled by the fluidized bed reactor and a lifting pipe reactor respectively, the problems that local hot spots, temperature runaway and particle adhesion can be easily caused in the strong heat release process of chlorination and chlorosulfonation are well solved, and meanwhile the method and device have the advantages of being easy to operate, high in raw material utilizing rate and the like.
Description
Technical field
The present invention relates to a kind of method and the device of preparing chlorosulfonated polyethylene, particularly relate to reaction unit and technique that a kind of gas solid method prepares chlorosulphonation vinylchlorid.
Background technology
Chlorosulfonated polyethylene is obtained through superchlorination and chlorosulfonation by Low Density Polyethylene or high density polyethylene(HDPE), for white or yellow elastic body, there are excellent ozone resistance, resistance to weathering, chemical resistance etc., good physical and mechanical properties, ageing-resistant performance, heat-resisting and lower temperature resistance, oil-proofness, flame resistivity, wear resistance and resistance to electrical insulating property, can be used for electric wire coating layer, cable edge layer, sebific duct, adhesive tape, automobile component, building waterproof coil, tank tank lining, offset plate, protective system etc., purposes is very extensive.
Gas solid method is the production technique of a kind of new chlorosulfonated polyethylene of development in recent years, compared with traditional solution method, gas solid method has reaction times short, the feature such as cost is low, it is little to pollute, technique is simple, shortcoming is that PE and CPE powder surface introduces chlorine and SULPHURYL CHLORIDE is not easy evenly, the quality of degree of crystallinity remaining influence CSM, simultaneously, system response temperature is wayward, subregion reaction heat not easily shifts out, and causes materials from bonding and coking, causes unstable product quality.
Chinese patent CN101759819 discloses a kind of device of preparing chlorosulfonated polyethylene by gas-solid phase method, its reaction unit comprises fluidized-bed, gas distribution grid, agitator, ultraviolet source, under UV-irradiation condition, material through fluidisation carries out sulfonation reaction, this device ultraviolet source is arranged at reactor head, region for fluidisation material bottom is difficult to fully and uniformly irradiate, cause reaction uneven, affect the quality of CSM, this reaction unit simultaneously, temperature in reaction process can not be solved completely wayward, reaction heat not easily shifts out, cause materials from bonding and these common problems of these gas solid methods of coking.
Chinese patent CN102698663 discloses a kind of fluidized-bed reactor of preparing chlorosulfonated polyethylene by gas-solid phase method, its reaction unit comprises fluidized-bed reaction main body, ultraviolet lamp Glass tubing group, gas pre-mixed room, pre-distributor, multi-layer gas grid distributor etc., this patent and Chinese patent reactor that CN101759819 mentions have similarity, all that ultraviolet source is set in the reactor, ultraviolet source is arranged in the middle part of reactor by this patent of difference, although improve to some extent in ultraviolet source position, but because reactor volume is larger, material can be caused equally to irradiate uneven.
Summary of the invention
The present invention want technical solution problem to be not enough for preparing chlorosulfonated polyethylene by gas-solid phase method, the reaction unit providing a kind of gas solid method to prepare chlorosulphonation vinylchlorid and technique, its concrete grammar is for adopting circulating fluidized bed mode, by material in fluidized-bed reactor and the cyclical operation of riser reactor two device, realize Matter Transfer fluidisation and complete chlorination, chlorosulfonation process simultaneously.
Its method technological process is:
1) first in fluidized-bed reactor, a certain amount of PE powder or CPE powder is added; chlorine and sulfur dioxide mixture gas is passed into by gas distribution grid by bottom fluidized-bed reactor; fully mix and fluidisation with the PE powder in fluidized-bed reactor or CPE powder; form gas-solid phase mixture; temperature in fluidized-bed reactor is controlled at 30 ~ 100 DEG C, fluidized-bed reactor pressure-controlling 0.05 ~ 0.15MPa;
2) gas-solid phase mixture enters riser reactor by the baiting valve bottom fluidized-bed reactor; riser reactor centre is provided with initiating device, gas-solid phase mixture generation priming reaction and preliminary chlorination under the active particle effect that initiating device excites, chlorosulfonation;
3) gas-solid phase mixture enters gas-solid separator by riser reactor, and after gas solid separation, solid phase PE powder or CPE powder enter fluidized-bed reactor and continue reaction, and gas phase portion uses through gas purifier process Posterior circle;
4) above-mentioned 1-3 step complete once cause and chlorination, chlorosulphonation process, continue circulation carry out, until after reaching chlorosulfonated polyethylene performance index, stop working cycle, replace discharging.
The invention provides reaction unit and technique that a kind of gas solid method prepares chlorosulphonation vinylchlorid, device has rational in infrastructure, easy and simple to handle, its device comprises the equipment connected successively: fluidized-bed reactor, discharge valve, riser reactor, gas-solid separator connect into closed circulation, it is characterized in that being operated by fluidized-bed reactor and riser reactor two device, realize Matter Transfer fluidisation and complete chlorination, chlorosulfonation process simultaneously.
The reaction unit of chlorosulfonated polyethylene prepared by above-mentioned a kind of gas solid method circulating fluidized bed, fluidized-bed reactor adopts jacketed type temperature control, control chlorination, chlorosulfonation process, be provided with initiating device in riser reactor, control chlorine, sulfurous gas excite process.
The reaction unit of chlorosulfonated polyethylene prepared by above-mentioned a kind of gas solid method circulating fluidized bed, and riser reactor adopts circular-gap reaction channel, and initiating device is arranged on the centre of riser tube.
The reaction unit of chlorosulfonated polyethylene prepared by above-mentioned a kind of gas solid method circulating fluidized bed, and the width of riser reactor annular space is 1-10mm.
The reaction unit of chlorosulfonated polyethylene prepared by above-mentioned a kind of gas solid method circulating fluidized bed, and the mode of excitation of initiating device adopts the mode that ultraviolet lamp, glow discharge, plasma medium electric discharge etc. are arbitrary or combine.
Advantage of the present invention and effect are:
1, fluidized-bed reactor and riser reactor two device working method, the initiation achieved, reaction two process decoupling zeros, Matter Transfer fluidisation completes chlorination, chlorosulfonation process simultaneously, well solves chlorination and this strong heat release inverse process of chlorosulphonation very easily causes hot localised points, temperature runaway and particle adhesion problem.
2, utilize circulating fluidized bed to prepare chlorosulfonated polyethylene, realize chlorine, sulfurous gas efficiency utilization, improve raw material availability.
3, riser reactor adopts circular-gap reaction channel, and initiating device is arranged on the centre of riser tube, can ensure that material evenly causes, thus ensures the homogeneity of chlorination and chlorosulphonation.
4, riser reactor adopts circular-gap reaction channel, and fully mixing and reaction heat shift out in time to be mutually conducive to gas-solid.
5, riser reactor adopts circular-gap reaction channel, does not have scale effect, as long as keep the width of annular space, just can ensure to cause effect, and the scale of device realizes by changing annular space internal-and external diameter value.
Accompanying drawing explanation
Fig. 1 is the reaction unit schematic diagram that a kind of gas solid method prepares chlorosulphonation vinylchlorid;
Fig. 2 is riser tube A-A sectional view.
Drawing reference numeral illustrates: 1-fluidized-bed reactor 2-baiting valve 3-gas purifier 4-admission passage 5-gas-solid separator 6-stirs 7-interchanger 8-gas distribution grid 9-blow-off valve 10-discharge valve 11-riser reactor 12-initiating device.
Embodiment
See accompanying drawing 1 and accompanying drawing 2, this device adopts fluidized-bed reactor and the operation of riser reactor two device, the initiation achieved, react two process decoupling zeros, specific operation process is as follows, raw material joins in fluidized-bed reactor 1 by baiting valve 2, chlorine is passed into by a certain percentage by admission passage 4, sulfur dioxide gas and nitrogen, mixed gas enters fluidized-bed reactor inside from fluidized reactor 1 bottom air inlet through gas distribution grid 8, raw material is under the effect of air-flow with stirring 6, realize Homogeneous phase mixing and the fluidisation of gas-solid phase, temperature in fluidized-bed reactor 1 is controlled at 30 ~ 100 DEG C, reactor pressure controls 0.05 ~ 0.15MPa, open the discharge valve 10 bottom fluidized-bed reactor 1, gas-solid phase mixture is under the blowing of mixed airflow, enter in riser reactor 11, under initiating device 12 acts on, there is provocative reaction, produce a large amount of free radicals, start chlorination, chlorosulfonation, gas-solid phase mixture by riser reactor 11 after gas-solid separator 5 carries out gas solid separation, solid phase returns in fluidized-bed reactor 1 and proceeds chlorination, chlorosulfonation, gas fraction and fluidized-bed reactor 1 Exhaust Gas use through gas purifier process Posterior circle, said process is in working cycle, fluidized-bed reactor 1 heats up by portion, by interchanger 7, temperature is controlled at 30 ~ 100 DEG C, react 30-120 minutes, fluidized-bed reactor 1 is let out to normal pressure, pass into nitrogen replacement reactive system, after completing displacement, open blow-off valve 9 discharging and can obtain chlorosulfonated polyethylene product.
Claims (6)
1. gas solid method prepares a reaction process for chlorosulphonation vinylchlorid, and its process steps is:
1) first in fluidized-bed reactor, a certain amount of PE powder or CPE powder is added, chlorine and sulfur dioxide mixture gas is passed into by gas distribution grid by bottom fluidized-bed reactor, fully mix and fluidisation with the PE powder in fluidized-bed reactor or CPE powder, form gas-solid phase mixture, temperature in fluidized-bed reactor is controlled at 30 ~ 100 DEG C, fluidized-bed reactor pressure-controlling 0.05 ~ 0.15MPa;
2) gas-solid phase mixture enters riser reactor by the baiting valve bottom fluidized-bed reactor, riser reactor centre is provided with initiating device, gas-solid phase mixture generation priming reaction and preliminary chlorination under the active particle effect that initiating device excites, chlorosulfonation;
3) gas-solid phase mixture enters gas-solid separator by riser reactor, and after gas solid separation, solid phase PE powder or CPE powder enter fluidized-bed reactor and continue reaction, and gas phase portion uses through gas purifier process Posterior circle;
4) above-mentioned 1-3 step complete once cause and chlorination, chlorosulphonation process, continue circulation carry out, until after reaching chlorosulfonated polyethylene performance index, stop working cycle, replace discharging.
2. the device realizing a kind of gas solid method according to claim 1 and prepare the technique of chlorosulphonation vinylchlorid, comprise the equipment connected successively: fluidized-bed reactor, baiting valve, riser reactor, gas-solid separator connect closed circulation, it is characterized in that material fluidized-bed reactor and riser reactor circulate complete simultaneously initiation and chlorination, chlorosulfonation process.
3. a kind of gas solid method according to claim 2 prepares the reaction unit of chlorosulphonation vinylchlorid, it is characterized in that fluidized-bed reactor adopts jacketed type temperature control, control chlorination, chlorosulfonation process, in riser reactor, be provided with initiating device, control chlorine, sulfurous gas causes process.
4. a kind of gas solid method according to claim 2 prepares the reaction unit of chlorosulphonation vinylchlorid, and it is characterized in that riser reactor adopts circular-gap reaction channel, initiating device is arranged on the centre of riser tube.
5. prepare the reaction unit of chlorosulphonation vinylchlorid according to the arbitrary described a kind of gas solid method of claim 2,4, it is characterized in that the width of the annular space of riser reactor is 1-10mm.
6. according to claim 2,4, a kind of gas solid method prepares the reaction unit of chlorosulphonation vinylchlorid, it is characterized in that the mode of excitation of initiating device adopts the mode that ultraviolet lamp, glow discharge, plasma medium electric discharge etc. are arbitrary or combine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610075569.3A CN105566527A (en) | 2016-02-03 | 2016-02-03 | Reaction device and technology for preparing chlorosulfonated chloroethylene through gas-solid phase method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610075569.3A CN105566527A (en) | 2016-02-03 | 2016-02-03 | Reaction device and technology for preparing chlorosulfonated chloroethylene through gas-solid phase method |
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| CN105566527A true CN105566527A (en) | 2016-05-11 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610075569.3A Pending CN105566527A (en) | 2016-02-03 | 2016-02-03 | Reaction device and technology for preparing chlorosulfonated chloroethylene through gas-solid phase method |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101759819A (en) * | 2009-12-22 | 2010-06-30 | 连云港金泰达橡胶材料有限公司 | Device for preparing chlorosulfonated polyethylene by gas-solid phase method |
| CN101831021A (en) * | 2010-05-10 | 2010-09-15 | 河北科技大学 | Device for preparing chlorinated polyvinyl chloride by gas-solid phase method and method thereof |
-
2016
- 2016-02-03 CN CN201610075569.3A patent/CN105566527A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101759819A (en) * | 2009-12-22 | 2010-06-30 | 连云港金泰达橡胶材料有限公司 | Device for preparing chlorosulfonated polyethylene by gas-solid phase method |
| CN101831021A (en) * | 2010-05-10 | 2010-09-15 | 河北科技大学 | Device for preparing chlorinated polyvinyl chloride by gas-solid phase method and method thereof |
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Application publication date: 20160511 |
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