CN101831021A - Device for preparing chlorinated polyvinyl chloride by gas-solid phase method and method thereof - Google Patents

Device for preparing chlorinated polyvinyl chloride by gas-solid phase method and method thereof Download PDF

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CN101831021A
CN101831021A CN201010165999.7A CN201010165999A CN101831021A CN 101831021 A CN101831021 A CN 101831021A CN 201010165999 A CN201010165999 A CN 201010165999A CN 101831021 A CN101831021 A CN 101831021A
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fluid bed
bed reactor
reactor
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CN101831021B (en
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王建英
胡永琪
张向京
刘玉敏
刘润静
郭欣欣
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Hebei University of Science and Technology
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Abstract

The invention belongs to the technical field of chemical processes and equipment, and relates to a device for preparing chlorinated polyvinyl chloride by a gas-solid phase method and a method thereof. The chlorinated polyvinyl chloride is prepared from polyvinyl chloride (PVC) and chlorine gas serving as raw materials in a dry state. The device comprises a riser reactor, a turbulent fluidized bed reactor, an upper connecting pipe and a lower connecting pipe, wherein the synthesis of the chlorinated polyvinyl chloride is performed in the riser reactor and the turbulent fluidized bed reactor; a chain initiation process is realized and chain transfer is finished by activating the chlorine gas with ultraviolet light, so that the whole process is decoupled into a quick process and a slow process, the chlorination of the materials is uniform, bonding and discoloration can be effectively prevented, the energy consumption is reduced and the operation is simplified; the device has the advantages of compact structure, high practicability and obvious improvement on the efficiency; hydrogen chloride separated from reaction tail gas can be recycled; and the whole process has no waste discharge.

Description

A kind of devices and methods therefor of preparing chlorinated polyvinyl chloride by gas-solid phase method
Technical field
The invention belongs to chemical technique and equipment technical field, relating to a kind of is the processing method and the device of raw material prepared in reaction chlorinated polyvinyl chloride (hereinafter to be referred as CPVC) under dry state with polyvinyl chloride (being called for short PVC) and chlorine.
Background technology
In the chlor-alkali industry, the chlorine about 60% that electrolytic process produces is used to produce polyvinyl chloride, and 20% raw material as organic chloride probably also has 20% residue.Because liquid chlorine is not easy to long-distance transport, there is the potential environmental problem in long-term storage.Along with the development of chlor-alkali industry, dissolving of chlorine more than needed is a problem being badly in need of solution.And utilize chlorine and pvc response, both can generate the chlorinated polyvinyl chloride product of high added value, but the superfluous chlorine that produces in the balanced production process again has good economic benefits and environmental benefit.
CPVC is with the further chlorination modified product of PVC.CPVC produces the method that generally adopts in the world three kinds: solvent method, water phase suspension, gas solid method.
Solvent method is the method that adopts the earliest, the technology comparative maturity, and its main processes is to carry out chlorination again after being dissolved in polyvinyl chloride resin in the halohydrocarbon, as US2996489.Because this method uses a large amount of organic solvents to exist problem of environmental pollution just progressively to be eliminated.Produce CPVC at present and generally adopt water phase suspension such as US5821304, US5981663, US6187868 etc., be powdery polyvinyl chloride resin is suspended in water or hydrogen chloride solution in, after adding auxiliary agent, adopt two sections chloridization process of low temperature (30~90 ℃) and high temperature (90~130 ℃).Adopt this legal system to be equipped with in the process of CPVC, explored some and improved the processing method of chlorination speed and product performance, as proposing to add organo-peroxide and UV-light initiation reaction among the US6197895; Introduce an amount of oxygen participation reaction among the US3506637 and all can improve chlorination speed and product performance.Aqueous-phase suspending technology also has a large amount of organic solvents to participate in reaction, and it is more to produce " three wastes ", and the equipment effective rate of utilization is lower, the last handling process complexity, and cost is higher relatively.Especially along with the CPVC demand increases day by day, a large amount of organic solvents are more and more sharp-pointed to the etching problem that equipment causes, and make to the having relatively high expectations of equipment, thereby increased production cost.
Gas-solid phase chlorination process is with the PVC powder, places in the fixed bed or fluidized-bed that has trap logical chlorine chlorination under external energy causes under the dry state situation.West Germany Lao Luner company at first proposed the imagination of gas-solid phase chlorination process in 1958, this method is compared with solution method with the water method, have and need not medium, technology and do not have the advantage that equipment corrosion, aftertreatment are simplified greatly and environmental pollution is light simply, substantially, have good development prospect.Human gas-solid phase stirring-type chlorination processs such as Qingdao University of Science and Technology's Yang Jinping prepare CPVC, derived PVC chlorating kinetic equation, have analyzed the reaction mechanism that chlorination by solid state method prepares CPVC.Though stirring tank technology flow process is simple, pollutant emission is little, heat-transfer effect is relatively poor, easily produces local superheating caking and product discoloration problem, is not suitable for scale operation.What US3532612 proposed produces CPVC with gas-solid phase fluidized bed process, adopts ultraviolet lamp and initiator catalyzed reaction, and temperature of reaction is lower, can realize the amplification production of CPVC, but this technical process complexity, not seeing has the industrialized report of realization.The Meng Yuedong of Hefei Inst. of Plasma Physics, Chinese Academy of Sciences and Xiong Xinyang etc. propose to adopt low-temperature plasma to prepare CPVC in its patent CN1749285A, make the chlorination of the quick gas-solid phase of PVC, but among the CPVC that makes cl content only up to 64.5%.
Summary of the invention
The present invention is for solving the problem in the present technology, provide a kind of simple and easy to do UV-light to cause the preparing chlorinated polyvinyl chloride by gas-solid phase method devices and methods therefor of (being called for short CPVC), it has technical process weak point, compact equipment, energy consumption is low, pollution is little characteristics.
The present invention is achieved by the following technical solutions:
A kind of device of preparing chlorinated polyvinyl chloride by gas-solid phase method, it comprises riser reactor, turbulent fluid bed reactor and last pipe connecting, following pipe connecting.
Described riser reactor comprises gas solid separation chamber, riser tube conversion zone and the unstripped gas inlet of the not isometrical cylindrical body that links to each other successively from top to bottom; One side on top, described gas solid separation chamber is provided with visor, and the inside center position of described gas solid separation chamber is provided with cyclonic separator; The top of described gas solid separation chamber is provided with the riser reactor tail gas outlet that links to each other with cyclonic separator; The outlet of riser reactor tail gas links to each other with the reaction gas inlet of recirculation blower and turbulent fluid bed reactor successively through pipeline; Be provided with some groups of riser reactor well heaters, some visors and some ultraviolet lamps in the described riser tube conversion zone; Upper end one side of described riser tube conversion zone is provided with pipe connecting, and is connected with the upside of turbulent fluid bed reactor; Described riser tube conversion zone lower end one side is provided with down pipe connecting, and is connected with the downside of turbulent fluid bed reactor; The described pipe connecting of going up is respectively equipped with valve with following pipe connecting; The lower end opposite side of described riser tube conversion zone is provided with discharge port, and inside, described riser tube conversion zone lower end is provided with gas distributor; The lower end of described riser reactor is provided with the unstripped gas inlet, is provided with air compartment between described gas distributor and the unstripped gas inlet.
Top one side of described turbulent fluid bed reactor is provided with the last pipe connecting that links to each other with riser tube conversion zone top, the top opposite side is provided with the solid feed inlet, the inside of described turbulent fluid bed reactor is provided with cyclonic separator, and the top of described turbulent fluid bed reactor is provided with the pneumatic outlet that links to each other with the top of cyclonic separator; Described pneumatic outlet links to each other with saturated aqueous common salt absorption tower, vitriol oil moisture eliminator, recirculation blower and unstripped gas inlet successively through pipeline; Well heater is positioned at the outside of turbulent fluid bed reactor, and described well heater top one side is provided with the heated oil inlet, and opposite side is provided with the heated oil outlet; Bottom one side of described turbulent fluid bed reactor is provided with the turbulent fluidized bed discharge port, and opposite side is provided with the following pipe connecting that links to each other with riser tube conversion zone bottom; The lower end of described turbulent fluid bed reactor is provided with the reaction gas inlet, is provided with air compartment between described gas distributor and the reaction gas inlet.
A kind of method of using said apparatus to prepare chlorinated polyvinyl chloride, it comprises the steps:
A. with screw feeder raw material PVC is joined turbulent fluid bed reactor by the solid feed inlet, to connect the last pipe connecting of turbulent fluid bed reactor and riser reactor, two valve opens on the following pipe connecting simultaneously, and have this moment a small amount of PVC under action of gravity, to flow in the riser reactor by pipe connecting under the turbulent fluid bed reactor warp;
B. with the unstripped gas inlet of unstripped gas from the riser reactor bottom, through air compartment, gas distributor feeds in the riser reactor, make the solid PVC particle generation fluidisation in the riser reactor, enter in the turbulent fluid bed reactor by last pipe connecting, simultaneously, the hydrogen chloride gas that reacts remaining chlorine and generation enters cyclonic separator through the gas solid separation chamber, after isolating the entrained solid particle, in the outlet of riser reactor tail gas, flow out, the solid particulate that is separated returns the bottom of riser tube conversion zone by the tremie pipe of cyclonic separator, effusive tail gas flows in the reaction gas inlet of turbulent fluid bed reactor as circulation gas after the recirculation blower pressurization in the outlet of riser reactor tail gas, by air compartment and gas distributor, make in the turbulent fluid bed reactor the solid PVC particle loosening wind action under the turbulence fluidisation takes place, and flow in the riser reactor gentle the depressing by following pipe connecting of gravity, make the effusive PVC amount of solid of turbulent fluid bed reactor equate (can judge) with the PVC amount of solid that turbulent fluid bed reactor flows into by regulated valve by the visor observation height of materials of riser reactor; Effusive tail gas is isolated the entrained solid particle through cyclonic separator from turbulent fluid bed reactor, again after pneumatic outlet enters the saturated aqueous common salt absorption tower and removes HCl, and unreacted Cl 2After vitriol oil moisture eliminator 26 dryings, enter the mouth with the incoming stock gas of unstripped gas by recirculation blower pressurization back as circulation gas;
C. open riser reactor well heater and ultraviolet lamp, make the temperature of riser reactor reach 60~120 ℃, simultaneously, feed heated oil from the heated oil inlet of well heater, make the turbulent fluid bed reactor temperature identical with the temperature of riser reactor, be 60~120 ℃, the heated oil after the heat exchange flows out from the heated oil outlet; In the riser reactor, under the exciting of UV-light, chlorine is decomposed into chlorine radical, and finish chain initiation process, and then the chlorination reaction of beginning polyvinyl chloride, finished the polyvinyl chloride of surface reaction, enter in the turbulent fluid bed reactor through last pipe connecting, further finish the chain transmittance process, realize degree of depth chlorination;
The chlorinated polyvinyl chloride particle that d. will reach the cl content requirement is directly got rid of from turbulent fluidized bed discharge port or discharge port, the particle that does not reach the cl content requirement circulates once more through riser tube conversion zone and turbulent fluid bed reactor, till reaching the cl content requirement.
The above-mentioned method for preparing chlorinated polyvinyl chloride, its described unstripped gas are pure chlorine or nitrogen or the mixed gas of the two; The particle diameter of described raw material PVC is at 25~500 μ m.
Working pressure in the above-mentioned method for preparing chlorinated polyvinyl chloride, described riser reactor is 0.05~0.1MPa, and the one way residence time of PVC particle in riser reactor is 0.5~2min.
The above-mentioned method for preparing chlorinated polyvinyl chloride, the working pressure of described turbulent fluid bed reactor are 0.05~0.1MPa, and the PVC particle one way residence time is 10~40min.
The beneficial effect that the present invention compared with prior art has is:
1. utilizing UV-activated chlorine and realize chain initiation process in riser tube, finish the chain transmission in turbulent bed, is two processes of speed with whole process decoupling zero, thereby make the material chlorination even, can effectively prevent bonding and variable color, reduce energy consumption, simplify operation.
2. UV-activated chlorine and chain initiation process are carried out in riser tube, gas-solid two-phase contact efficiency height, and the gas-solid white heat is fast, and it is strong that heat moves in and out ability, thereby reaction is carried out smoothly.
3. by orthogonal directions many ultraviolet lamps are set on the inherent horizontal plane of riser reactor, ultraviolet lamp is evenly distributed, and illumination is abundant, thereby improves photocatalysis efficiency greatly.
4. be equivalent to the effect of baffle plate on the inherent horizontal plane of riser reactor by many ultraviolet lamps of orthogonal directions setting, can effectively eliminate the channel and the joint of ultra-fine grain when fluidisation and emerge in large numbers and resemble.
5. the turbulent fluidized bed diameter is greater than riser tube conversion zone diameter, and the particle residence time is long, helps slow chain transmittance process and fully carries out.
6. the present invention is a circulating fluidized bed system, and the gas velocity regulation range is wide, and turndown ratio is big, and output is bigger.
7. this reacts and is gas-solid phase reaction, and organic solvent-free participates in, and aftertreatment is simple, and is pollution-free substantially.
In a word, the present invention have that technical process is short, energy consumption is low, reaction is even, smooth operation and the characteristics of control easily.Utilize this processing method and device can make raw material PVC be converted into the CPVC of high added value, and realize the recycling of chlorine.
Description of drawings
Fig. 1 is the structural representation of the device of preparing chlorinated polyvinyl chloride by gas-solid phase method of the present invention.
The explanation of symbol in the accompanying drawing:
1, riser reactor tail gas outlet; 2a, 2b, cyclonic separator; 3, gas solid separation chamber; 4, riser reactor well heater; 5, riser reactor; 6, riser tube conversion zone; 7, visor; 8, ultraviolet lamp; 9, discharge port; 10, gas distributor; 11, air compartment; 12, unstripped gas inlet; 13, go up pipe connecting; 14, following pipe connecting; 15, valve; 16, turbulent fluid bed reactor; 17, pneumatic outlet; 18, solid feed inlet; 19, well heater; 20, heated oil inlet; 21, heated oil outlet; 22, turbulent fluidized bed discharge port; 23, gas distributor; 24, reaction gas inlet; 25a, 25b, recirculation blower; 26, vitriol oil moisture eliminator; 27, saturated aqueous common salt absorption tower
Embodiment
Specific embodiments of the present invention is described in detail with reference to the accompanying drawings.
As Fig. 1 is the structural representation of the device of preparing chlorinated polyvinyl chloride by gas-solid phase method of the present invention.
The device of a kind of preparing chlorinated polyvinyl chloride by gas-solid phase method of the present invention, it comprises riser reactor 5, turbulent fluid bed reactor 16 and last pipe connecting 13, following pipe connecting 14.
Described riser reactor 5 comprises gas solid separation chamber 3, riser tube conversion zone 6 and the unstripped gas inlet 12 of the not isometrical cylindrical body that links to each other successively from top to bottom; One side on 3 tops, described gas solid separation chamber is provided with visor 7, and the inside center position of described gas solid separation chamber 3 is provided with cyclonic separator 2a; The top of described gas solid separation chamber 3 is provided with the riser reactor tail gas outlet 1 that links to each other with cyclonic separator 2a; The outlet 1 of riser reactor tail gas links to each other with the reaction gas inlet 24 of recirculation blower 25b and turbulent fluid bed reactor 16 successively through pipeline; Be provided with some groups of riser reactor well heaters 4, some visors 7 and some ultraviolet lamps 8 in the described riser tube conversion zone 6; Upper end one side of described riser tube conversion zone 6 is provided with pipe connecting 13, and is connected with the upside of turbulent fluid bed reactor 16; Described riser tube conversion zone 6 lower ends one side is provided with down pipe connecting 14, and is connected with the downside of turbulent fluid bed reactor 16; The described pipe connecting 13 of going up is respectively equipped with valve 15 with following pipe connecting 14; The lower end opposite side of described riser tube conversion zone 6 is provided with discharge port 9, and inside, described riser tube conversion zone 6 lower end is provided with gas distributor 10; The lower end of described riser reactor 5 is provided with unstripped gas inlet 12, is provided with the 11a of air compartment between described gas distributor 10 and the unstripped gas inlet 12.
Top one side of described turbulent fluid bed reactor 16 is provided with the last pipe connecting 13 that links to each other with riser tube conversion zone 6 tops, the top opposite side is provided with solid feed inlet 18, the inside of described turbulent fluid bed reactor 16 is provided with cyclonic separator 2b, and the top of described turbulent fluid bed reactor 16 is provided with the pneumatic outlet 17 that links to each other with the top of cyclonic separator 2b; Described pneumatic outlet 17 links to each other with saturated aqueous common salt absorption tower 27, vitriol oil moisture eliminator 26, recirculation blower 25a and unstripped gas inlet 12 successively through pipeline; Well heater 19 is positioned at the outside of turbulent fluid bed reactor 16, and described well heater 19 tops one side is provided with heated oil inlet 20, and opposite side is provided with heated oil outlet 21; Bottom one side of described turbulent fluid bed reactor 16 is provided with turbulent fluidized bed discharge port 22, and opposite side is provided with the following pipe connecting 14 that links to each other with riser tube conversion zone 6 bottoms; The lower end of described turbulent fluid bed reactor 16 is provided with reaction gas inlet 24, is provided with the 11b of air compartment between described gas distributor 23 and the reaction gas inlet 24.
A kind of method of using said apparatus to prepare chlorinated polyvinyl chloride, it comprises the steps:
A. with screw feeder raw material PVC is joined turbulent fluid bed reactor 16 by solid feed inlet 18, to connect the last pipe connecting 13 of turbulent fluid bed reactor 16 and riser reactor 5 simultaneously, down two valves 15 on the pipe connecting 14 are opened, have this moment a small amount of PVC under action of gravity by turbulent fluid bed reactor 16 through under pipe connecting 14 flow in the riser reactors 5;
B. with the unstripped gas inlet 12 of unstripped gas from the riser reactor bottom, through the 11a of air compartment, gas distributor 10 feeds in the riser reactor 5, make the solid PVC particle generation fluidisation in the riser reactor 5, enter in the turbulent fluid bed reactor 16 by last pipe connecting 13, simultaneously, the hydrogen chloride gas that reacts remaining chlorine and generation enters cyclonic separator 2a through gas solid separation chamber 3, after isolating the entrained solid particle, in riser reactor tail gas outlet 1, flow out, the solid particulate that is separated returns the bottom of riser tube conversion zone 6 by the tremie pipe of cyclonic separator 2a, effusive tail gas flows in the reaction gas inlet 24 of turbulent fluid bed reactor 16 as circulation gas after recirculation blower 25b pressurization in the outlet 1 of riser reactor tail gas, by 11b of air compartment and gas distributor 23, make in the turbulent fluid bed reactor 16 the solid PVC particle loosening wind action under the turbulence fluidisation takes place, and flow in the riser reactor 5 gentle the depressing by following pipe connecting 14 of gravity, make turbulent fluid bed reactor 16 effusive PVC amount of solid equate (the visor 7 observation height of materials by riser reactor 5 are judged) with the PVC amount of solid that turbulent fluid bed reactor 16 flows into by regulated valve 15; Effusive tail gas is isolated the entrained solid particle through cyclonic separator 2b from turbulent fluid bed reactor, after pneumatic outlet 17 entered saturated aqueous common salt absorption tower 27 and removes HCl, unreacted Cl2 entered the mouth 12 by recirculation blower 25a pressurization back with the incoming stock gas of unstripped gas as circulation gas through vitriol oil moisture eliminator 26 dry backs again;
C. open riser reactor well heater 4 and ultraviolet lamp 8, make the temperature of riser reactor reach 60~120 ℃, simultaneously, feed heated oil from the heated oil inlet 20 of well heater 19, make the turbulent fluid bed reactor temperature identical with the temperature of riser reactor, be 60~120 ℃, the heated oil after the heat exchange flows out from heated oil outlet 21; In the riser reactor 5, under the exciting of UV-light, chlorine is decomposed into chlorine radical, and finish chain initiation process, and then the chlorination reaction of beginning polyvinyl chloride, finished the polyvinyl chloride of surface reaction, enter in the turbulent fluid bed reactor through last pipe connecting, further finish the chain transmittance process, realize degree of depth chlorination;
The chlorinated polyvinyl chloride particle that d. will reach the cl content requirement is directly got rid of from turbulent fluidized bed discharge port 22 or discharge port 9, the particle that does not reach the cl content requirement circulates once more through riser tube conversion zone 6 and turbulent fluid bed reactor 16, till reaching the cl content requirement.
The above-mentioned method for preparing chlorinated polyvinyl chloride, its described unstripped gas are pure chlorine or nitrogen or the mixed gas of the two; The particle diameter of described raw material PVC is at 25~500 μ m.
Working pressure in the above-mentioned method for preparing chlorinated polyvinyl chloride, described riser reactor is 0.05~0.1MPa, and the one way residence time of PVC particle in riser reactor is 0.5~2min.
The above-mentioned method for preparing chlorinated polyvinyl chloride, the working pressure of described turbulent fluid bed reactor are 0.05~0.1MPa, and the PVC particle one way residence time is 10~40min.
Embodiment 1:
In apparatus of the present invention as shown in Figure 1, adopting particle diameter is raw material at the PVC of 100~150 μ m, and unstripped gas is pure chlorine, pure chlorinated with chlorine, chlorination temperature is 100~110 ℃, working pressure is 0.05MPa in the riser reactor, and the particle one way residence time is 1min, and working pressure is 0.08MPa in the turbulent fluid bed reactor, the particle one way residence time is 10min, behind the reaction 1h, the cl content of products C PVC is 68%, satisfies the requirement of CPVC content fully.
Embodiment 2:
In apparatus of the present invention as shown in Figure 1, adopting particle diameter is raw material at the PVC of 150~200 μ m, unstripped gas is chloride 30% chlorine and nitrogen mixture body, and chlorination temperature is 110~120 ℃, and working pressure is 0.05MPa in the riser reactor, the particle one way residence time is 2min, working pressure is 0.06MPa in the turbulent fluid bed reactor, and the particle one way residence time is 20min, behind the reaction 1.5h, the cl content of products C PVC is 69%, satisfies the requirement of CPVC content fully.
Embodiment 3:
In reaction unit as shown in Figure 1, adopting particle diameter is raw material at the PVC of 150~200 μ m, unstripped gas is chloride 30% chlorine and nitrogen mixture body, and chlorination temperature is 110~120 ℃, and working pressure is 0.06MPa in the riser reactor, the particle one way residence time is 0.5min, working pressure is 0.08MPa in the turbulent fluid bed reactor, and the particle one way residence time is 10min, behind the reaction 1.5h, the cl content of products C PVC is 67%, satisfies the requirement of CPVC content fully.

Claims (5)

1. the device of a preparing chlorinated polyvinyl chloride by gas-solid phase method is characterized in that:
It comprises riser reactor (5), turbulent fluid bed reactor (16) and last pipe connecting (13), following pipe connecting (14);
Described riser reactor (5) comprises gas solid separation chamber (3), riser tube conversion zone (6) and the unstripped gas inlet (12) of the not isometrical cylindrical body that links to each other successively from top to bottom; One side on top, described gas solid separation chamber (3) is provided with visor (7), and the inside center position of described gas solid separation chamber (3) is provided with cyclonic separator (2a); The top of described gas solid separation chamber (3) is provided with the riser reactor tail gas outlet (1) that links to each other with cyclonic separator (2a); Riser reactor tail gas outlet (1) links to each other with the reaction gas inlet (24) of recirculation blower (25b) and turbulent fluid bed reactor (16) successively through pipeline; Be provided with some groups of riser reactor well heaters (4), some visors (7) and some ultraviolet lamps (8) in the described riser tube conversion zone (6); Upper end one side of described riser tube conversion zone (6) is provided with pipe connecting (13), and is connected with the upside of turbulent fluid bed reactor (16); Described riser tube conversion zone (6) lower end one side is provided with down pipe connecting (14), and is connected with the downside of turbulent fluid bed reactor (16); Described upward pipe connecting (13) and following pipe connecting (14) are respectively equipped with valve (15); The lower end opposite side of described riser tube conversion zone (6) is provided with discharge port (9), and described riser tube conversion zone (6) inside, lower end is provided with gas distributor (10); The lower end of described riser reactor (5) is provided with unstripped gas inlet (12), is provided with air compartment (11a) between described gas distributor (10) and the unstripped gas inlet (12);
Top one side of described turbulent fluid bed reactor (16) is provided with the last pipe connecting (13) that links to each other with riser tube conversion zone (6) top, the top opposite side is provided with solid feed inlet (18), the inside of described turbulent fluid bed reactor (16) is provided with cyclonic separator (2b), and the top of described turbulent fluid bed reactor (16) is provided with the pneumatic outlet (17) that links to each other with the top of cyclonic separator (2b); Described pneumatic outlet (17) links to each other with saturated aqueous common salt absorption tower (27), vitriol oil moisture eliminator (26), recirculation blower (25a) and unstripped gas inlet (12) successively through pipeline; Well heater (19) is positioned at the outside of turbulent fluid bed reactor (16), and described well heater (19) top one side is provided with heated oil inlet (20), and opposite side is provided with heated oil outlet (21); Bottom one side of described turbulent fluid bed reactor (16) is provided with turbulent fluidized bed discharge port (22), and opposite side is provided with the following pipe connecting (14) that links to each other with riser tube conversion zone (6) bottom; The lower end of described turbulent fluid bed reactor (16) is provided with reaction gas inlet (24), is provided with air compartment (11b) between described gas distributor (23) and the reaction gas inlet (24).
2. a method of using the described device of claim 1 to prepare chlorinated polyvinyl chloride is characterized in that it comprises the steps:
A. with screw feeder raw material PVC is joined turbulent fluid bed reactor (16) by solid feed inlet (18), to connect the last pipe connecting (13) of turbulent fluid bed reactor (16) and riser reactor (5) simultaneously, down two valves (15) on the pipe connecting (14) are opened, have this moment a small amount of PVC under action of gravity by turbulent fluid bed reactor (16) in pipe connecting (14) inflow riser reactor (5) down;
B. with the unstripped gas inlet (12) of unstripped gas from the riser reactor bottom, through air compartment (11a), gas distributor (10) feeds in the riser reactor (5), make the solid PVC particle generation fluidisation in the riser reactor (5), enter in the turbulent fluid bed reactor (16) by last pipe connecting (13), simultaneously, the hydrogen chloride gas that reacts remaining chlorine and generation enters cyclonic separator (2a) through gas solid separation chamber (3), after isolating the entrained solid particle, in riser reactor tail gas outlet (1), flow out, the solid particulate that is separated returns the bottom of riser tube conversion zone (6) by the tremie pipe of cyclonic separator (2a), effusive tail gas flows in the reaction gas inlet (24) of turbulent fluid bed reactor (16) as circulation gas after recirculation blower (25b) pressurization in riser reactor tail gas outlet (1), by air compartment (11b) and gas distributor (23), make in the turbulent fluid bed reactor (16) the solid PVC particle loosening wind action under the turbulence fluidisation takes place, and flow in the riser reactor (5) gentle the depressing by following pipe connecting (14) of gravity, by regulated valve (15) the effusive PVC amount of solid of turbulent fluid bed reactor (16) is equated with the PVC amount of solid of turbulent fluid bed reactor (16) inflow; Effusive tail gas is isolated the entrained solid particle through cyclonic separator (2b) from turbulent fluid bed reactor, again after pneumatic outlet (17) enters saturated aqueous common salt absorption tower (27) and removes HCl, unreacted Cl2 through the dry back of vitriol oil moisture eliminator (26) as circulation gas by recirculation blower (25a) pressurization back with the incoming stock gas of unstripped gas enter the mouth (12);
C. open riser reactor well heater (4) and ultraviolet lamp (8), make the temperature of riser reactor reach 60~120 ℃, simultaneously, feed heated oil from the heated oil inlet (20) of well heater (19), make the turbulent fluid bed reactor temperature identical with the temperature of riser reactor, be 60~120 ℃, the heated oil after the heat exchange flows out from heated oil outlet (21); In the riser reactor (5), under the exciting of UV-light, chlorine is decomposed into chlorine radical, and finish chain initiation process, and then the chlorination reaction of beginning polyvinyl chloride, finished the polyvinyl chloride of surface reaction, enter in the turbulent fluid bed reactor through last pipe connecting, further finish the chain transmittance process, realize degree of depth chlorination;
The chlorinated polyvinyl chloride particle that d. will reach the cl content requirement is directly got rid of from turbulent fluidized bed discharge port (22) or discharge port (9), the particle that does not reach the cl content requirement circulates once more through riser tube conversion zone (6) and turbulent fluid bed reactor (16), till reaching the cl content requirement.
3. the method for preparing chlorinated polyvinyl chloride as claimed in claim 2 is characterized in that, described unstripped gas is pure chlorine or nitrogen or the mixed gas of the two; The particle diameter of described raw material PVC is at 25~500 μ m.
4. the method for preparing chlorinated polyvinyl chloride as claimed in claim 2 is characterized in that, the working pressure in the described riser reactor is 0.05~0.1MPa, and the one way residence time of PVC particle in riser reactor is 0.5~2min.
5. the method for preparing chlorinated polyvinyl chloride as claimed in claim 2 is characterized in that, the working pressure of described turbulent fluid bed reactor is 0.05~0.1MPa, and the PVC particle one way residence time is 10~40min.
CN2010101659997A 2010-05-10 2010-05-10 Device for preparing chlorinated polyvinyl chloride by gas-solid phase method and method thereof Expired - Fee Related CN101831021B (en)

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CN102502589A (en) * 2011-11-09 2012-06-20 清华大学 Device and method for continuously preparing high-purity single/double-wall carbon nano tubes
CN103497264A (en) * 2013-09-29 2014-01-08 中国平煤神马能源化工集团有限责任公司 Reaction system and method for intermittent production of chlorinated polyvinyl chloride
CN104250324A (en) * 2014-07-16 2014-12-31 杭州新元化工技术开发有限公司 Gas-solid phase reaction method for preparation of chlorinated polyvinyl chloride
CN104395359A (en) * 2013-03-29 2015-03-04 株式会社钟化 Production method and production device for chlorinated vinyl chloride-based resin
CN104607114A (en) * 2014-07-01 2015-05-13 新疆兵团现代绿色氯碱化工工程研究中心(有限公司) Apparatus and process for producing chlorinated high polymer
CN105566527A (en) * 2016-02-03 2016-05-11 新疆兵团现代绿色氯碱化工工程研究中心(有限公司) Reaction device and technology for preparing chlorosulfonated chloroethylene through gas-solid phase method
CN105693894A (en) * 2016-04-22 2016-06-22 杭州电化集团有限公司 Device and method for producing chlorinated polyvinyl chloride
CN107115829A (en) * 2017-05-16 2017-09-01 北京清诚华宇科技有限公司 Laser induced recirculating fluidized bed produces the device and method of haloflex
CN107417814A (en) * 2017-06-16 2017-12-01 新疆兵团现代绿色氯碱化工工程研究中心(有限公司) A kind of chlorinated high polymers process units and technique for controlling reacting gas concentration respectively
CN108948238A (en) * 2018-08-29 2018-12-07 江苏德邦工程有限公司 A kind of method preparing chliorinated polyvinyl chloride and its preparation facilities
CN109369829A (en) * 2018-10-26 2019-02-22 山东高信化学股份有限公司 The injection molding preparation method of high-performance chlorinated polyvinyl chloride
CN114950283A (en) * 2022-06-24 2022-08-30 洛阳融惠化工科技有限公司 Fluidized reaction system for coating surfaces of ultrafine particles and using method thereof

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Cited By (20)

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CN102502589B (en) * 2011-11-09 2014-01-01 清华大学 Device and method for continuously preparing high-purity single/double-wall carbon nano tubes
CN102502589A (en) * 2011-11-09 2012-06-20 清华大学 Device and method for continuously preparing high-purity single/double-wall carbon nano tubes
CN104395359B (en) * 2013-03-29 2016-03-16 株式会社钟化 The manufacture method of chlorinated vinyl chloride-based resin and manufacturing installation
CN104395359A (en) * 2013-03-29 2015-03-04 株式会社钟化 Production method and production device for chlorinated vinyl chloride-based resin
CN103497264A (en) * 2013-09-29 2014-01-08 中国平煤神马能源化工集团有限责任公司 Reaction system and method for intermittent production of chlorinated polyvinyl chloride
CN103497264B (en) * 2013-09-29 2016-07-06 中国平煤神马能源化工集团有限责任公司 The response system of a kind of Batch Process chliorinated polyvinyl chloride and method
CN104607114B (en) * 2014-07-01 2017-02-15 新疆兵团现代绿色氯碱化工工程研究中心(有限公司) Apparatus and process for producing chlorinated high polymer
CN104607114A (en) * 2014-07-01 2015-05-13 新疆兵团现代绿色氯碱化工工程研究中心(有限公司) Apparatus and process for producing chlorinated high polymer
CN104250324A (en) * 2014-07-16 2014-12-31 杭州新元化工技术开发有限公司 Gas-solid phase reaction method for preparation of chlorinated polyvinyl chloride
CN105566527A (en) * 2016-02-03 2016-05-11 新疆兵团现代绿色氯碱化工工程研究中心(有限公司) Reaction device and technology for preparing chlorosulfonated chloroethylene through gas-solid phase method
CN105693894A (en) * 2016-04-22 2016-06-22 杭州电化集团有限公司 Device and method for producing chlorinated polyvinyl chloride
CN107115829B (en) * 2017-05-16 2019-10-25 北京清诚华宇科技有限公司 The device and method of laser induced recirculating fluidized bed production haloflex
CN107115829A (en) * 2017-05-16 2017-09-01 北京清诚华宇科技有限公司 Laser induced recirculating fluidized bed produces the device and method of haloflex
CN107417814A (en) * 2017-06-16 2017-12-01 新疆兵团现代绿色氯碱化工工程研究中心(有限公司) A kind of chlorinated high polymers process units and technique for controlling reacting gas concentration respectively
CN108948238A (en) * 2018-08-29 2018-12-07 江苏德邦工程有限公司 A kind of method preparing chliorinated polyvinyl chloride and its preparation facilities
CN108948238B (en) * 2018-08-29 2023-06-30 江苏德邦工程有限公司 Method for preparing chlorinated polyvinyl chloride and preparation device thereof
CN109369829A (en) * 2018-10-26 2019-02-22 山东高信化学股份有限公司 The injection molding preparation method of high-performance chlorinated polyvinyl chloride
CN109369829B (en) * 2018-10-26 2021-04-13 山东高信化学股份有限公司 Preparation method of high-performance chlorinated polyvinyl chloride for injection molding
CN114950283A (en) * 2022-06-24 2022-08-30 洛阳融惠化工科技有限公司 Fluidized reaction system for coating surfaces of ultrafine particles and using method thereof
CN114950283B (en) * 2022-06-24 2023-06-16 洛阳融惠化工科技有限公司 Fluidization reaction system for superfine particle surface coating and application method thereof

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