CN104607114B - Apparatus and process for producing chlorinated high polymer - Google Patents
Apparatus and process for producing chlorinated high polymer Download PDFInfo
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- CN104607114B CN104607114B CN201410308204.1A CN201410308204A CN104607114B CN 104607114 B CN104607114 B CN 104607114B CN 201410308204 A CN201410308204 A CN 201410308204A CN 104607114 B CN104607114 B CN 104607114B
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- 229920000642 polymer Polymers 0.000 title claims abstract description 153
- 238000000034 method Methods 0.000 title claims abstract description 57
- 230000008569 process Effects 0.000 title abstract description 30
- 239000007789 gas Substances 0.000 claims abstract description 77
- 238000005660 chlorination reaction Methods 0.000 claims abstract description 50
- 238000006243 chemical reaction Methods 0.000 claims abstract description 32
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000460 chlorine Substances 0.000 claims abstract description 19
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 9
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 9
- 230000004913 activation Effects 0.000 claims abstract description 3
- 238000012546 transfer Methods 0.000 claims description 22
- 239000012535 impurity Substances 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 11
- 230000009467 reduction Effects 0.000 claims description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 230000004044 response Effects 0.000 claims description 6
- 238000006073 displacement reaction Methods 0.000 claims description 5
- 230000003321 amplification Effects 0.000 claims description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 4
- 238000003199 nucleic acid amplification method Methods 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 238000007790 scraping Methods 0.000 claims description 3
- 206010020843 Hyperthermia Diseases 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 230000036031 hyperthermia Effects 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims 1
- 235000007164 Oryza sativa Nutrition 0.000 claims 1
- 238000004026 adhesive bonding Methods 0.000 claims 1
- 235000009566 rice Nutrition 0.000 claims 1
- 235000012239 silicon dioxide Nutrition 0.000 claims 1
- 239000000377 silicon dioxide Substances 0.000 claims 1
- 238000005243 fluidization Methods 0.000 abstract description 15
- 238000003756 stirring Methods 0.000 abstract description 12
- 230000033001 locomotion Effects 0.000 abstract description 3
- 238000007599 discharging Methods 0.000 abstract description 2
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 abstract 2
- 239000012495 reaction gas Substances 0.000 abstract 2
- 230000005284 excitation Effects 0.000 abstract 1
- 239000011261 inert gas Substances 0.000 abstract 1
- 230000001737 promoting effect Effects 0.000 abstract 1
- 239000012530 fluid Substances 0.000 description 13
- 238000004519 manufacturing process Methods 0.000 description 12
- 230000003197 catalytic effect Effects 0.000 description 11
- 238000006555 catalytic reaction Methods 0.000 description 9
- 238000002156 mixing Methods 0.000 description 9
- 150000002835 noble gases Chemical class 0.000 description 8
- 230000003134 recirculating effect Effects 0.000 description 8
- 239000008187 granular material Substances 0.000 description 7
- 229910052756 noble gas Inorganic materials 0.000 description 7
- 229920000915 polyvinyl chloride Polymers 0.000 description 7
- 239000004800 polyvinyl chloride Substances 0.000 description 7
- 239000003708 ampul Substances 0.000 description 6
- 108010066057 cabin-1 Proteins 0.000 description 6
- 230000008859 change Effects 0.000 description 6
- 238000010276 construction Methods 0.000 description 6
- 239000010453 quartz Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 230000005012 migration Effects 0.000 description 5
- 238000013508 migration Methods 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 230000033228 biological regulation Effects 0.000 description 4
- 239000008246 gaseous mixture Substances 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000008878 coupling Effects 0.000 description 3
- 238000010168 coupling process Methods 0.000 description 3
- 238000005859 coupling reaction Methods 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 239000005543 nano-size silicon particle Substances 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 241000208340 Araliaceae Species 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 2
- 235000003140 Panax quinquefolius Nutrition 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 235000008434 ginseng Nutrition 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- -1 polyethylene Polymers 0.000 description 2
- 238000012805 post-processing Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000004709 Chlorinated polyethylene Substances 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000003851 corona treatment Methods 0.000 description 1
- 238000006392 deoxygenation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229920001596 poly (chlorostyrenes) Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
-
- 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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
- B01J19/122—Incoherent waves
- B01J19/123—Ultraviolet light
-
- 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
- B01J8/1818—Feeding of the fluidising gas
- B01J8/1827—Feeding of the fluidising gas the fluidising gas being a reactant
-
- 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
- B01J8/26—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 with two or more fluidised beds, e.g. reactor and regeneration installations
-
- 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
- B01J8/38—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 with fluidised bed containing a rotatable device or being subject to rotation or to a circulatory movement, i.e. leaving a vessel and subsequently re-entering it
- B01J8/384—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 with fluidised bed containing a rotatable device or being subject to rotation or to a circulatory movement, i.e. leaving a vessel and subsequently re-entering it being subject to a circulatory movement only
- B01J8/388—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 with fluidised bed containing a rotatable device or being subject to rotation or to a circulatory movement, i.e. leaving a vessel and subsequently re-entering it being subject to a circulatory movement only externally, i.e. the particles leaving the vessel and subsequently re-entering it
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention provides an apparatus and process for producing a chlorinated high polymer. According to the invention, plasma or ultraviolet lamps are used to excite chlorine gas so as to prepare the chlorinated high polymer. Under the action of fluidization gas and fluidization-aiding gas, the chlorinated high polymer is produced by a pretreated high polymer under the excitation of plasma or ultraviolet light through stirring and heating, wherein the fluidization gas is composed of pretreated chlorine gas and hydrogen chloride gas or inert gas in proportion. Due to the gradient control of the chlorination reaction heat, two or more fluidized bed reactors are installed in the apparatus and connected by risers which are easy to adjust length and each of which is internally provided with an ultraviolet light tube or a plasma discharging device, wherein the risers are mainly used for exciting reaction gas, prolonging gas activation time, dissipating heat and promoting uniform reaction. The high polymer and the reaction gas circulate between the two fluidized bed reactors through the risers, so the phenomenon of uneven chlorination caused by backmixing occurred in single-bed fluidization can be avoided and the phenomenon of non-smooth movement of materials caused by the height restriction of a high polymer layer can be overcome; and thus, reaction heat is better controlled, and the high polymer meets the requirement of uniform chlorine content.
Description
Technical field
The invention belongs to Chemical Manufacture manufactures field, especially a kind of device producing chlorinated high polymers and technique.
Background technology
Existing chlorinated polymeric production technology mainly includes solwution method, water phase suspension, gas solid method.Due to solvent method
Produce chlorinated polymeric and can produce harmful in a large number and heavy damage atmospheric ozone layer organic solvent, thus at present by
Manufacturer is phased out both at home and abroad.Water phase suspension production technology is that current most enterprises produce chlorinated polyethylene and chlorination
The main method of polrvinyl chloride.But water phase suspension production technology needs substantial amounts of water body resource as carrier, to China's hydropenia
The water source in area causes larger waste and pollution, thus the new clean and effective type production technology of exploitation is to solve root problem
Crucial.Gas solid method is to be in circulating fluid bed reactor and riser reactor Corvic under dry state situation
Continuous flowing, carries out depth chlorination with chlorine reaction and chliorinated polyvinyl chloride is obtained., due to its process is simple, equipment is rotten for gas solid method
Erosion is little, is widely paid close attention to the features such as low production cost.
Existing gas solid method is individually with ultraviolet light or plasma-catalytic, is a kind of conventional, promising height
Polymers chlorination catalytic way.Ultraviolet catalytic can reduce reaction temperature, and energy stabilization, small power consumption, and plasma-catalytic enters
One step reduces reaction temperature, at room temperature just can be with catalytic chlorination, but power consumption is higher, more difficult assurance on energy stability.Specially
Profit 201010165999.7 proposes and adopts recirculating fluidized bed with the gas solid method system of ultraviolet catalytic in riser reactor
The method of standby chliorinated polyvinyl chloride, only recirculating fluidized bed and riser reactor two-way air inlet, there is no blanking auxiliary air passage, hold
Easily there is blanking blockage, uniform blanking is poor；It is susceptible to material air-teturning mixed phenomenon it is impossible to ensure chlorination uniformity simultaneously, by
In chlorination value to a certain extent when, this reaction cannot be carried out the effective transfer of heat for Fast exothermic process.Patent
200910092928.6《Method and the equipment of chliorinated polyvinyl chloride prepared by low temperature plasma recirculating fluidized bed》Propose using low
Isothermal plasma can activate the feature of chlorine and polyvinyl chloride surface simultaneously, achieve and efficiently excite polychlorostyrene second in down-flow fluidized bed using ECT
The process of alkene chlorination reaction, and realize the process that surface chlorine internally rotates migration further in riser and turbulent bed, from
And whole chlorination process is decoupled as two steps of speed, production efficiency is substantially better than ultraviolet chlorination and water phase suspension chlorination mistake
Journey；But material is in concentrated phase flow regime in descending-bed reactor, solid-gas ratio is high, gas shape after corona treatment
The chlorine radical becoming is few, occurs the probability of chlorination reaction little, increased plant maintenance operation, and utilization rate of equipment and installations is low, and wait from
Sub- relative temperature is high, and this reaction mid-term is reacted for Fast exothermic, and therefore heat is unable to effective transfer.Patent
201110061421.1《The method and apparatus that low temperature plasma circulation fluidized bed continuously produces chliorinated polyvinyl chloride》Propose using low
The method that chliorinated polyvinyl chloride is produced in isothermal plasma catalysis, realizes the quick chlorination of PVC in recirculating fluidized bed, two groups simultaneously
Fluidized-bed reactor operated in turn realizes continuous production, and such one is that of avoiding due to reactor shutdowns, the life that discharging is brought
The problems such as product efficiency reduces；On the other hand blower fan and exhaust gas processing device etc. can be avoided to stop restart, save the energy and disappear
Consumption, extends equipment life, but there is also material in descending-bed reactor and be in concentrated phase flow regime, and solid-gas ratio is high, and chlorine occurs
The probability changing reaction is little, and chlorination is uneven, material easily blocks, back-mixing, and temperature is unable to effective control, increases plant maintenance simultaneously
Workload.
Content of the invention
It is an object of the invention to provide a kind of device producing chlorinated high polymers and technique, specifically utilize two or
Plural recirculating fluidized bed, with being easy to adjustment length and being internally provided with the riser of plasma or uviol lamp and carry out even
Connect, by stirring and fluidizing the combination of device of air；Using two or more plasma or uviol lamps of being internally provided with
Riser is attached recirculating fluidized bed lower end and top, in conjunction with chuck；Solve the problems such as back-mixing, catalysis time control, heat transfer,
Realize chlorination uniformly, heat transfer is rapid, heat transfer uniformity is consistent between granule, purpose that is extending the catalytic action time；Meanwhile, using taking out
Vacuum equipment it is achieved that chloride reaction before and after process；Clean manufacturing, riser employs circular-gap structure, successfully solves
Heat transfer in the transfer of high polymer and the course of reaction of having determined.
Technical scheme is as follows：A kind of device producing chlorinated high polymers, by the fluidized-bed reaction coupling successively
Device 11, riser 9, regulator 13, vacuum equipment 12, gas knot screen 8, heating system 6；Wherein use riser 9 order
Connect two or more fluidized-bed reactors 11, can effectively adjust polymer reaction when high polymer passes through riser 9
When temperature, reacting gas can be made to be sufficiently mixed with high polymer, the setting of two fluidized-bed reactors 11, make in high polymer from one
After platform fluidized-bed reactor 11A to another fluidized-bed reactor 11B, do not remain in First fluidized-bed reactor 11A, from
And avoid back-mixing, ensure that the high polymer of same batch is catalyzed number of times under the catalytic environment of plasma or uviol lamp identical simultaneously,
Catalysis time is as close as regulator 13 is connected in fluidized-bed reactor 11, for adjusting fluidized-bed reactor 11
Pressure, vacuum equipment 12 is connected in fluidized-bed reactor 11, for providing fluidized-bed reactor 11 negative pressure, gas knot screen 8
It is connected in high polymer upstream end, for gas purification, deoxygenation, heating system 6 is connected in fluidized-bed reactor 11 and riser 9,
For adjusting response system thermal balance.
Technical process for said apparatus can be carried out in accordance with the following steps：
A, reacting gas are chlorine, hydrogen chloride gas and noble gases（Noble gases are：It is not involved in the gas of this technological reaction
Body, this paper abbreviation noble gases）Proportioning forms, and carries out remove impurity, deoxidation by gas knot screen 8 to gas, is added with heating system 6
Hot gas；Wherein, chlorine and hydrogen chloride volume proportion are 0.3-0.9；Deoxidation reaches below 500ppm；Gas is heated to 25-160
DEG C, Stress control is in 0.01-0.1MPa；After gas passes through gas knot screen 8, entered by fluidisation device of air 5 and fluidizer device of air 7
Enter response system；Fluidisation device of air 5 and fluidizer device of air 7 are provided with fluidisation device of air.
B, high polymer enter raw material cabin 1 through pretreatment, enter amplification section 2 and fall into fluidized-bed reactor A after drying；Its
In, high polymer can be polyethylene, polrvinyl chloride, polypropylene etc.；Pretreated particle diameter be 80-150 μm, and remove attached collection
Gas on grain；After high polymer enters fluidized-bed reactor A, carry out reacting gas displacement, so that reacting gas is incorporated, attached collect
Grain surface and inside.
C, in the presence of the fluidizer gas from the fluidisation fluidized gas of device of air 5 and fluidizer device of air 7, using stirring 3 stream
Change high polymer, heating system 6 fluid bedreactors 11 chuck carries out being heated to 25-160 DEG C simultaneously, using regulator 13,
Adjust fluidized-bed reactor 11A, the pressure reduction at fluidized-bed reactor 11B two ends, in the presence of pressure reduction, high polymer is anti-by fluid bed
Answer device 11A, fluidized-bed reactor 11B is entered by riser 9；Wherein, by being arranged on the ultraviolet lamp tube 19 within riser 9
Activation fluidizer gas and high polymer, make high polymer that chlorination to occur；High polymer passes through be sequentially connected in series two risers of setting
9, extend gas, high polymer soak time, and convenient regulation, reinforcement are conducted heat and promote polymer reaction uniform；Continue to reconcile stream
The pressure reduction of fluidized bed reactor 11A and B, realizes the circulation between fluidized-bed reactor 11A, B of high polymer and gas, circulates every time
All the high polymer in fluidized-bed reactor is completely fed to another fluidized-bed reactor 11, it is to avoid single fluidized-bed reactor 11
The generation of air-teturning mixed phenomenon, high polymer is in two or more fluidized-bed reactors and lifting in-pipe, until high polymer
Chlorinity reaches requirement, and the motion of high polymer is not limited by bed depth, can lift in-pipe in two or more, improve
Chlorination uniformity.
After d, chlorination value reach requirement, using vacuum equipment 12, fluid bedreactors carry out Negative pressure, remove absorption
Residual gas on reactant；After Negative pressure finishes, it is passed through air, enter line replacement；Finish rear high polymer and be transported to finished product
Feed bin 10.
Fluidized-bed reactor 11 as above is the two or more continuous metaplasias being in series, realizing high polymer
Produce, strengthen the back-mixing of high polymer that conducts heat, avoids.
Stirring as above is provided with scrapes wall construction 20 and chiller 21；It is bonded in fluidisation using scraping wall construction removing
High polymer on bed reactor 11 inwall, prevents localized hyperthermia from occurring；Refrigerating device inside enhances high polymer heat transfer simultaneously.
Riser 9 as above is annular space structure, and outer tube chuck 18 is set it is ensured that high polymer chlorination uniform
Property, strengthen heat transfer and reaction temperature controls.
Riser 9 as above is internal to arrange ultraviolet lamp tube 19, outside setting outer tube chuck 18, quartz ampoule 17 and outer tube
Form annular space between chuck 18.
Electrode 15 in the internal setting plasma of another form of riser 9 as above, outside set gradually etc. from
Sub- external electrode 16, outer tube chuck 18, the riser 9 with plasma discharge apparatus for the composition, quartz ampoule 17 and outer tube chuck 18 it
Between formed annular space.
Fluidized-bed reactor 11 as above is provided with amplification section 2, and in running, bottom is close phase state, amplifies section and is
Dilute phase state, riser is also dilute phase, and ultra-vioket radiation area is also dilute phase state, is easy to ultraviolet and causes catalysis.
Technical process as above, high polymer passes through to be dilute phase state during riser 9, chlorination early stage fluidizer temperature degree is high
In high polymer temperature, chlorination later stage fluidizer temperature degree is less than high polymer temperature.
Technical process as above, fluidizer gas as the high polymer in conveying hoisting pipe 9 and controls temperature.
Technical process as above, for ensureing the control of temperature, riser 9 can arrange outer tube chuck 18, for controlling
Temperature in riser 9 for the high polymer.
For solving back-mixing, the problems such as catalysis time controls, heat controls, realize chlorination uniformly, heat transfer is rapid, pass between granule
Thermal uniformity is consistent, purpose that is extending the catalytic action time；The present invention can also be with following art scheme：Including the stream coupling successively
Fluidized bed reactor 11, riser 9, regulator 13, vacuum equipment 12, gas knot screen 8, heating system 6；Wherein with 6
Riser 9 is linked in sequence more than two fluidized-bed reactors 11,9 points two kinds of riser, a kind of riser of interior ultraviolet modulated structure
14, one kind does not install ultraviolet lamp tube 19, for extending riser 9, two kinds of risers 9 is separated connection, passes through riser in high polymer
Temperature during polymer reaction can effectively be adjusted when 9, so that reacting gas is sufficiently mixed with high polymer, more than two fluid beds are anti-
Answer the setting of device 11, make in high polymer after a fluidized-bed reactor 11A to another fluidized-bed reactor 11B, before
Not remaining in platform fluidized-bed reactor 11A, thus avoiding back-mixing, ensureing the high polymer of same batch in plasma or ultraviolet simultaneously
Under the catalytic environment of lamp, catalysis number of times is identical, and catalysis time is as close as riser 9 outer wall setting chuck is used for temperature control
System.Add nano-calcium carbonate, nano silicon, nano aluminium oxide etc. can eliminate in its technical process in entering high polymer
The nanometer powder of high polymer electrostatic, remaining is with last scheme.
Device as above, electrode 15 in plasma, plasma external electrode 16, quartz ampoule 17, outer tube chuck 18 and
Plasma power supply, connection successively forms plasma discharge apparatus, and that is, a kind of circular-gap dielectric barrier discharge plasma fills
Put.
The principle of the present invention be using riser reactor material be dilute phase feature, by control riser flow and
The temperature of its fluidizer gas air-flow, the stirring structure of fluidized-bed reactor, the set location of ultraviolet lamp tube, the structure shape of reactor
Formula, process of raw material etc. controlling the reaction temperature of high polymer granule, thus avoiding the quick chlorination of high polymer and producing reunion.
The present invention implement beneficial effect be：
1st, after chlorination initial stage and chlorination finish, all using vacuum equipment, remove the gas of attached collection in high polymer, further
Improve chlorination efficiency, and make finished product material without alkali cleaning generic operation, be more beneficial for environmental protection.
2nd, catalytic unit using plasma and ultraviolet light compound mode, the chlorination initial stage adopts plasma method, drops further
Low chlorination temperature, the chlorination later stage adopts ultraviolet method, reduces energy consumption.
3rd, the riser being combined using two or more, and fluidized-bed reactor A, the design of B, strengthen dissipating of system
Heat and heat transfer, being capable of more preferable controlling reaction temperature.Extend the response time, it is to avoid the easy temperature runaway of single bed recirculating fluidized bed, high
The easy back-mixing of polymers material, the shortcomings of reaction is uneven；And using circular-gap design structure and jacket structured, be more beneficial for controlling reaction
Temperature and production scale are amplified.
4th, using under dilute phase conditions, temperature control is carried out to the granule in high polymer chlorination process in chlorination process, thus controlling
The temperature of W-response processed, has reached the uniformity needed for material.
Brief description
Fig. 1 is W-response flow process and reaction unit schematic diagram；
Fig. 2 is riser schematic diagram；
Fig. 3 is riser internal structure schematic diagram；
Fig. 4 scrapes wall construction and internal heat transfer structural representation for stirring；
Fig. 5 is many cascaded structure schematic diagrams；
Fig. 6 is flow process and the reaction unit schematic diagram of single fluidised bed reactor；
Fig. 7 is horizontal reactor schematic device.
Drawing reference numeral：1 is raw material cabin;2 is to amplify section；3 is stirring；4 is reactor jacket；5 is fluidisation device of air；6 are
Heating system；7 is fluidizer device of air；8 is gas knot screen；9 is riser；10 is finished product bin；11、11A、11B、11C、
11D is fluidized-bed reactor, fluidized-bed reactor A, B, C, D；12 is vacuum equipment；13 is regulator；14 is ultraviolet lamp tube
The riser of structure；15 is electrode in plasma；16 is plasma external electrode；17 is quartz ampoule；18 is outer tube chuck；19 is purple
Outer fluorescent tube；20 is to scrape wall construction；21 is chiller；22 is auger；23 is horizontal reactor.
Specific embodiment
Embodiment 1：
With reference to Figure of description 1；Raw material cabin 1 is pressurizeed, high polymer flows into after amplifying section 2 and falls into fluidized-bed reactor
11A.Open vacuum equipment 12, high polymer is carried out with evacuation process, remove the gaseous impurity of attached collection on high polymer.Chlorine and chlorine
Change hydrogen or the gaseous mixture of noble gases carries out remove impurity, deoxidation, and heating by device 8, gas heating-up temperature is 20-
130℃.Gas after heating, enters fluidized-bed reactor 11A by fluidizing device of air 5, high polymer is fluidized, prechlorination
After 10-60 minute, open heating system 6, fluid bedreactors and riser are heated, temperature is 20-130 DEG C.Pass through
To 11A, fluidized-bed reactor 11B carries out pressure regulation to regulator 13, improves the internal pressure of fluidized-bed reactor 11A.Help
Gas body enters into lifting bottom of the tube by fluidizer device of air 7, and in the presence of pressure reduction, powder flows into riser 9, opens riser
Internal plasma discharge apparatus and ultraviolet lamp tube 19, activate to high polymer and gas.High polymer is completely into fluidisation
After bed reactor 11B, change the direction of A and B pressure reduction and fluidizer gas, high polymer begins to flow to fluidized-bed reactor 11A, completes one
Individual circulation.After high polymer temperature rise is to 60-80 DEG C, opens ultraviolet lamp tube, activated using ultraviolet, circulate through multiple.Treat
After high polymer chlorinity meets requirement, close fluidized gas and fluidizer gas, using the chlorine to absorption on high polymer for the vacuum equipment 12,
Hydrogen chloride and noble gases carry out remove impurity.After remove impurity finishes, it is passed through air, high polymer inside is filled with, after finishing, by height
Polymers is unloaded to finished product bin 10, completes chlorination and remove impurity.
Embodiment 2：
With reference to Figure of description 5；Raw material cabin 1 is pressurizeed, high polymer flows into after amplifying section 2 and falls into fluidized-bed reactor
11A.Open vacuum equipment 12, high polymer is carried out with evacuation process, remove the gaseous impurity of attached collection on high polymer.Chlorine and chlorine
Change hydrogen or the gaseous mixture of noble gases carries out remove impurity, deoxidation by gas knot screen 8, gas heating-up temperature is 25-
160℃.Gas after heating, enters fluidized-bed reactor 11A by fluidizing device of air 5, high polymer is fluidized, prechlorination
After 10-60 minute, open heating system 6, fluid bedreactors and riser are heated, temperature is 25-160 DEG C.Pass through
Regulator 13 fluid bedreactors 11A carry out pressure regulation, improve the internal pressure of fluidized-bed reactor A.Fluidizer gas
Lifting bottom of the tube is entered into by fluidizer device of air 7, in the presence of pressure reduction, high polymer flows into riser 9, opens in riser 9
The plasma discharge apparatus in portion and ultraviolet lamp tube 19, activate to high polymer and gas.High polymer is completely into fluid bed
After reactor 11B, continue through the good reacting gas of addition proportioning and fluidized, the inside reaching high polymer chlorination reaction is moved
Move.After fluidized-bed reactor A feeding finishes, continue to feed to fluidized-bed reactor A from raw material cabin 1, carry out high polymer prechlorination.
Adjust fluidized-bed reactor B, the pressure reduction of C, high polymer flows to fluidized-bed reactor 11C by riser 9, and high polymer is in fluid bed
Carry out the internal migration of high polymer chlorination reaction in reactor C.After finishing, adjust fluidized-bed reactor C and fluidized-bed reactor D
Pressure, complete migration and the fluidisation of high polymer, after chlorination finishes, taken out by vacuum equipment 12 fluid bedreactors D
Application of vacuum, removes remaining hydrogen chloride on high polymer for the attached collection and chlorine.It is passed through air, after completing displacement, high polymer is squeezed into
Finished bin 10.Repeat the above steps, realize continuous prodution.
Embodiment 3：
With reference to Figure of description 1 and 2；The difference of embodiment 3 and embodiment 1,2 is the structure of riser 9, one
It is the riser 14 of ultraviolet lamp tube mechanism, another is electrode 15 and plasma external electrode 16 and quartz ampoule in plasma
17th, outer tube chuck 18 forms the circular-gap plasma producing apparatus as shown in Figure of description 2,3.
Embodiment 4：
With reference to Figure of description 1-5, the present embodiment and above example difference are：Pretreatment to high polymer,
Remove impurity, screening, heating were all carried out before entering fluidized-bed reactor 11A, and riser 9 is linked in sequence 5 fluidized-bed reactors
11, high polymer proceeding through riser 9 and subsequent fluidized bed reactor 11, reaches after entering First fluidized-bed reactor 11
Chlorination carries out post processing after requiring, and enters back into finished product bin 10.When First high polymer is completely into second or subsequently arbitrary
During one fluidized-bed reactor 11, high polymer that pretreatment completes can entrance fluidized-bed reactor 11 successively, thus reaching
Continuous production.
Embodiment 5：
With reference to Figure of description 6, the pretreatment of the present embodiment high polymer is arbitrary with post processing and embodiment 1-4 identical, no
Be only to be coupled with riser 9 with a fluidized-bed reactor 11, high polymer from fluidized-bed bottom out, by riser 9
In the presence of fluidizer device of air 7, enter from the top of fluidized-bed reactor 11, through the circulation of appropriate time and the control of temperature
System, carries out evacuation process by vacuum equipment 12 fluid bedreactors 11, removes remaining chlorination on high polymer for the attached collection
Hydrogen and chlorine.It is passed through air, after completing displacement, high polymer is squeezed into finished bin 10.
Embodiment 6：
With reference to Figure of description 2,3,4,6, the present embodiment include coupling successively 1, raw material cabin;5th, fluidize device of air；6、
Heating system；7th, fluidizer device of air；8th, gas knot screen；9th, riser；10th, finished product bin；11st, fluidized-bed reactor；Its
Middle use circular-gap riser（Inside riser 9, ultraviolet lamp tube 19 is not installed, quartz ampoule 17 is only installed）Connection fluidized-bed reaction
The outlet at bottom of device 11 and top inlet, ultraviolet lamp tube 19 is arranged on fluidized-bed reactor 11 inwall, and fluidizer device of air 7 is out
Constant temperature gas is carried high polymer secretly and is passed through riser 9, and when high polymer flows in riser 9, fluidizer gas and high polymer granule are fully mixed
Close, with setting stirring 3 inside the temperature during gas regulation high polymer particle reaction of constant temperature, fluidized-bed reactor, stirring 3 sets
It is equipped with and scrapes wall construction 20 and chiller 21, make high polymer be unlikely to overheated and be bonded on the wall of fluidized-bed reactor 11.Its work
Raw material cabin 1 is pressurizeed by skill process, and high polymer flows into after amplifying section 2 and falls into fluidized-bed reactor 11.Chlorine and hydrogen chloride gas
The gaseous mixture of body or noble gases carries out remove impurity, deoxidation by gas knot screen 8, and gas heating-up temperature is 25-160 DEG C.
Gas after heating, enters fluidized-bed reactor 11 by fluidizing device of air 5, high polymer is fluidized, prechlorination 10-60 divides
Zhong Hou, opens heating system 6, and fluid bedreactors and riser are heated, and temperature is 25-160 DEG C.Fluidizer gas is by helping
Gas device 7 enters into lifting bottom of the tube, and in the presence of pressure reduction, high polymer flows into riser 9, opens ultraviolet lamp tube 19, right
High polymer and gas are activated.Continue through the good reacting gas of addition proportioning to be fluidized, reach high polymer chlorination reaction
Internal migration.High polymer in fluidized-bed reactor 11 continuously flows into upper inlet from lower end through riser 9, until
Complete migration and the fluidisation of high polymer, using riser 9 and its pass through fluidized gas controlling reaction temperature, reaction rate；Chlorine
Change after finishing, remove remaining hydrogen chloride on high polymer for the attached collection and chlorine.It is passed through air, after completing displacement, high polymer is squeezed into
Finished bin 10.Repeat the above steps, realize continuous prodution.
Embodiment 7：
With reference to Figure of description 2,3,4,6, the present embodiment is with the difference of embodiment 6, and ultraviolet lamp tube 19 is used instead
For ultraviolet lamp bead, on multiple blades scraping wall construction 20 being arranged in stirring, its technical process is similar to Example 6, no
Be for controlling reaction temperature fluidizer gas temperature in the reaction the later stage be less than fluidized-bed reactor 11 temperature, in high polymer
The materials such as nano silicon, nano-calcium carbonate, nano aluminium oxide are added in raw material, for eliminating the electrostatic of high polymer generation,
Prevent the generation of viscous wall.Technical process is with embodiment 6.
Embodiment 8：
The present invention may also provide implementation below, specifically reactor wall setting ultraviolet lamp tube 9, with being easy to
The riser 9 of adjustment length is attached, by stirring the combination of 3 and fluidisation device of air 5；Carried using two or more
Riser 9, connects recirculating fluidized bed lower end and top, solves the problems such as back-mixing, catalysis time control, heat transfer, realizes chlorination uniformly,
Heat transfer is rapid, heat transfer uniformity is consistent between granule, purpose that is extending the catalytic action time；Meanwhile, using vacuum extractor 12, real
The process before and after chloride reacts, clean manufacturing are showed；Riser employs circular-gap structure, improves the radiating surface in riser
Long-pending, accelerate movement velocity in riser for the high polymer, successfully solve heat in the transfer of high polymer and course of reaction and turn
Move.With embodiment 6 in technical process, in high polymer, except for the difference that add nano silicon, nano-calcium carbonate, nano oxidized
The materials such as aluminum, for eliminating the electrostatic of high polymer generation, prevent the generation of viscous wall, solve material uniformity.
Embodiment 9：
Ginseng Figure of description 7, the present invention may also provide implementation below, and specifically reactor dilute-phase zone is interior
Wall arranges the horizontal reactor 23 of ultraviolet lamp tube 19, by the combination of auger 22 and fluidisation device of air 5；Solve back-mixing, urge
Change the problems such as time control, heat transfer, realize chlorination uniformly, heat transfer is rapid, heat transfer uniformity is consistent, extend catalytic action between granule
The purpose of time；Meanwhile, using vacuum extractor 12, the process before and after chloride reaction, clean manufacturing are realized；Technical process will
Raw material cabin 1 is pressurizeed, and high polymer flows into horizontal reactor, opens vacuum equipment 12, carries out evacuation process to high polymer, go
Gaseous impurity except collection attached on high polymer.The gaseous mixture of chlorine and hydrogen chloride gas or noble gases is removed by device 8
Miscellaneous, deoxidation, and heating, gas heating-up temperature is 20-130 DEG C.Gas after heating, enters Horizontal counter by fluidizing device of air 5
Answer device, high polymer is fluidized, after prechlorination 10-60 minute, open heating system 6, horizontal reactor is heated, temperature
Spend for 20-130 DEG C.Open reactor ultraviolet lamp tube 19, high polymer and gas are activated.Effect in auger 22 power
Under, high polymer continuously moves from left to right, continuous chlorination, and the high polymer of low order end enters knot screen, after remove impurity finishes,
High polymer is unloaded to finished product bin 10, completes chlorination and remove impurity.In this embodiment, the setting of horizontal reactor enables material to exist
In one reactor, existing dilute-phase zone has emulsion zone again, and solves catalysis in same reactor and react, and ultraviolet is installed
In dilute-phase zone, solve the problems, such as chlorination uniformity using auger 22 and fluidisation device of air 5, thus avoiding vertical reactor
Installation difficulty is big, and investment is high, and the problem more than equipment is moreover it is possible to make its technique continuous and stable production.
Embodiment 10：
Ginseng Figure of description 7, embodiments of the present invention as different from Example 9, are arranged on auger 22 leaf
Ultraviolet lamp bead, in the presence of ultra-vioket radiation is passed through on stirring side, prevents material from because of ultra-vioket radiation, asking of adhesion uviol lamp wall occurring
Topic；Its technical process is same as Example 9.
Claims (9)
1. a kind of produce chlorinated high polymers technique be：
A, the chlorine for 0.3-0.9 for the volume ratio and hydrogen chloride gas are carried out deoxidation remove impurity post-heating to 25-160 DEG C, by fluidizing
Device of air and fluidizer device of air enter response system；
B, the high polymer after pretreatment and drying enter and amplify paragraph fluidized bed reactor A, carry out reacting gas displacement,
So that gas is incorporated and attached collect high polymer particle surface and inside；
C, in the presence of fluidized gas and fluidizer gas, using agitating device fluidize high polymer, simultaneously heating system to each fluidize
Bed reactor jacket is heated, and opening regulator makes fluidized-bed reactor A and fluidized-bed reactor B produce pressure reduction, Gao Ju
Thing, by fluidized-bed reactor A, enters fluidized-bed reactor B by the riser of jacketed；By being arranged within riser
Plasma or ultraviolet lamp tube is arbitrary or the two activation fluidizer gas and high polymer, makes high polymer that chlorination to occur；By lifting
Pipe, extends gas and high polymer soak time, strengthens heat transfer and promotes polymer reaction uniform；Continue to adjust fluidized-bed reactor
The pressure reduction of A and B, realizes high polymer in fluidized-bed reactor A, the circulation between B, circulation is all by fluidized-bed reactor every time
High polymer is completely fed to another fluidized-bed reactor, and high polymer is in two or more fluidized-bed reactors and lifting
In-pipe, until high polymer chlorinity reaches requirement, riser is linked in sequence more than two fluidized-bed reactors；
After d, chlorination value reach requirement, remove residual gas on high polymer for the absorption, then enter line replacement, go out finished product.
2. a kind of technique producing chlorinated high polymers as described in claim 1 is it is characterised in that fluidized-bed reactor is two
More than it is in series, realize the continuous prodution of high polymer.
3. a kind of technique producing chlorinated high polymers as described in claim 1 scrapes wall it is characterised in that agitating device is provided with
Structure and chiller；Remove, using scraping wall device, the high polymer being bonded on fluidized-bed reactor inwall, prevent localized hyperthermia
Occur；Chiller enhances the heat transfer of high polymer simultaneously.
4. a kind of technique producing chlorinated high polymers as described in claim 1 is it is characterised in that arrange ultraviolet inside riser
Fluorescent tube, outside setting outer tube chuck, be annular space structure it is ensured that the uniformity of high polymer chlorination, strengthen heat transfer and reaction temperature
Degree controls.
5. by a kind of arbitrary described technique producing chlorinated high polymers of claim 1,4 it is characterised in that setting inside riser
Put electrode in plasma, outside sets gradually plasma external electrode, outer tube chuck.
6. a kind of technique producing chlorinated high polymers as described in claim 1, fluidized-bed reactor is equipped with amplification section, runs
During bottom be close phase state, amplifications section be dilute phase state, riser be dilute phase state.
7. a kind of technique producing chlorinated high polymers as described in claim 1, high polymer passes through to be dilute phase state during riser,
Chlorination early stage fluidizer temperature degree is higher than high polymer temperature, and chlorination later stage fluidizer temperature degree is less than high polymer temperature.
8. a kind of technique producing chlorinated high polymers as described in claim 1, for ensureing the control of temperature, riser can be arranged
Outer tube chuck, for controlling temperature in riser for the high polymer.
9. a kind of technique producing chlorinated high polymers as described in claim 1, before chlorination starts, adds in high polymer raw material and receives
Rice silicon dioxide, nano-calcium carbonate, nano aluminium oxide be arbitrary or two or more material, for eliminating the electrostatic of high polymer generation,
Prevent high polymer from gluing the generation of wall.
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