CN205347297U - Can be used to synthetic alkoxylate reaction unit of unsaturated polyether - Google Patents
Can be used to synthetic alkoxylate reaction unit of unsaturated polyether Download PDFInfo
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- CN205347297U CN205347297U CN201521062572.9U CN201521062572U CN205347297U CN 205347297 U CN205347297 U CN 205347297U CN 201521062572 U CN201521062572 U CN 201521062572U CN 205347297 U CN205347297 U CN 205347297U
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Abstract
The utility model provides a can be used to synthetic alkoxylate reaction unit of unsaturated polyether. The circulation circuit that the device was contacted and is formed including alkoxylate reactor (6), circulating pump (10) and heat exchanger (11) order still includes to concatenate mixed cauldron (4) between heat exchanger (11) and alkoxylate reactor (6), alkoxylate reactor (6) interior evenly distributed has along many reaction pipeline (8) that the axial set up, reaction pipeline (8) is formed by connecting major diameter pipeline (15) and minor diameter pipeline (16) in turn, the internal diameter of major diameter pipeline (15) and minor diameter pipeline (16) than be 1.2~3, length is than being 1~10. The utility model discloses the material mix abundant, to polyether viscosity increase insensitive, mass transfer heat transfer efficiency high, can be used to the alkoxylate reaction of synthetic unsaturated polyether.
Description
Technical field
This utility model belongs to chemical industry equipment and manufactures field, specifically a kind of alkoxylation device that can be used for unsaturated polyether synthesis.
Background technology
Polycarboxylate water-reducer is after the high efficiency water reducing agent that naphthalene sulfonic salt water reducer is representative, and the third generation high-performance water reducing agent developed has the advantages such as volume is little, water-reducing rate is high, function of slump protection is good.General is that raw material is formed by radical polymerization with unsaturated carboxylic acid monomer by unsaturated polyether, and in water reducer, the quality accounting of polyethers is very big, and the performance of water reducer is had material impact by its quality.
Polyethers is mainly synthesized by alkoxylation under catalyst action by initiator and epoxyalkane, and the factor affecting course of reaction mainly includes catalyst, reaction temperature, reaction pressure, mass transfer, heat transfer etc..(Wu Sanhua, domestic and international ethoxylation device technique technology and prospect [J]. the tenth time, whole nation industrial surface activity agent Technological Economy and application and development proceeding, 2001), it is reflected in the quality aspect of the polyether product of final preparation, including hydroxyl value or molecular weight, molecular weight distribution, degree of unsaturation and poly-alkyl diol content (invalid component) etc..
The reaction temperature of the industrialized production of unsaturated polyether and reaction pressure are generally strict controlled in certain scope, and catalyst is typically chosen base catalyst such as metallic sodium, sodium hydride and Feldalat NM etc..Owing to synthesis unsaturated polyether needs to use the initiator containing unsaturated double-bond, in the process of synthesizing polyether, there is the situation of double bond inefficacy or polymerization, so alkoxylate equipment is had significantly high requirement.The mass transfer of alkoxylate equipment and heat transfer are the key factors affecting unsaturated polyether alkoxylation, relevant with production efficiency of equipment on the one hand, ensure that the degree of unsaturation of polyether product on the other hand.Additionally, the epoxy monomer concentration of residual reduces in polyethers building-up process, safety and the significant (Ji Fengyu of polyethers quality control to production process, the design [J] of ethoxylation still. Liaoning chemical industry, 1993, (3), 48-49).
Domestic for different process conditions with product design demand at present, intermittent operation or continuous operation can be adopted, the alkoxylate equipment being suitable for is generally divided into the reactor types such as autoclave, tubular type, falling film type, nebulisation cycle formula and spray circuits formula (in sword elder brother etc., the progress [J] of alkoxylated ethoxylated reactor. chemical propellant and macromolecular material, 2015,13 (2), 8-27).
Development along with domestic and international polyethers synthetic technology, improvement and optimization to alkoxylation equipment are constantly carrying out always, main research direction is in strengthening mass transfer and heat transfer, by measures such as the energy consumptions in the production efficiency of raising unit equipment and reduction course of reaction, improve the quality of polyether product, reduce production cost.
Along with static mixer (Fan Cunliang, static mixer application [J] in ethoxylation. chemical equipment technology, 1998, 19 (5), 4-7), injection reactor (Yuan Shaoming etc., injection reactor and application [J] thereof. daily chemical industry, 2003, 33 (1), 40-43), and with one heart the parts such as mozzle or structural member are introduced into alkoxylation device, devise a variety of follow-on alkoxylation device both at home and abroad, including internal recycle tank reactor (US6838061), outer circulation tank reactor (EP2678374), reactor (the Qin Yong that injection reactor and autoclave combine, brief talk the development trend [J] of China's ethoxylation production technology. household chemicals science, 2014, 37 (11), 1-6), by the V of injection reactor and circulation spraying coupling for Press reactor etc., significantly enhance the mass transfer effect between material, there is higher production efficiency.
Above reactor achieves good effect in improving reactor mass-and heat-transfer, but the Some features of reactor itself limits their range of application.BUSS reactor and Press reactor are not suitable for dystectic solid initiator; the high viscosity of high molecular weight polyether is very sensitive; and tank reactor is applicable to the synthesis of small lot, high molecular, high viscous polyether; but mass-and heat-transfer effect is relatively poor, the double bond protection of unsaturated polyether is unfavorable.
Utility model content
This utility model provides a kind of alkoxylation device that can be used for unsaturated polyether synthesis, and mixing of materials is fully, insensitive to the increase of polyethers viscosity, mass-and heat-transfer efficiency high, can be used for synthesizing the alkoxylation of unsaturated polyether.
The described alkoxylation device that can be used for unsaturated polyether synthesis includes alkoxylation device, the closed circuit that circulating pump and heat exchanger order are connected in series, also include the mixing kettle being serially connected between heat exchanger and alkoxylation device, it is provided with mechanical stirring device in described mixing kettle, top is provided with initiator/catalyst feeds and the outer circulation loop material charging aperture being connected with heat exchanger discharging opening, bottom is provided with alkylene oxide monomer charging aperture and is connected to the mixing kettle discharging opening at alkoxylation device top, it is provided with atomising device in the material charging aperture of described outer circulation loop, many axially disposed reacting pipes it are evenly distributed with in described alkoxylation device, described reacting pipe is alternately formed by connecting by large-diameter pipeline and small diameter pipeline, the internal diameter (D/d) of large-diameter pipeline and small diameter pipeline is 1.2～3, length ratio (L1/L2) is 1～10.
In the present invention, reacting pipe is alternately connected to form by large-diameter pipeline and small diameter pipeline, can be provided with changeover portion between large-diameter pipeline and small diameter pipeline, and the length of described changeover portion counts small diameter pipeline length.
This utility model is as follows for the concrete operations of alkoxylation:
Pretreatment stage: mixing kettle, alkoxylation device, circulating pump, heat exchanger and pipeline dry in advance；
The stage of reaction: add initiator, catalyst from initiator/catalyst feeds to mixing kettle, be then shut off initiator/catalyst feeds；Mixing kettle is warming up to 60～100 DEG C in churned mechanically process, to mixing kettle, alkylene oxide monomer is passed into from epoxyalkane charged monomer charging aperture, reaction to be polymerized starts (i.e. pressure reduction in mixing kettle, temperature raises), open the pipe valve (alkoxylation device preheats in advance) connecting alkoxylation device, ON cycle pump and heat exchanger；Keep alkoxylation actuator temperature reaction temperature (reaction temperature is generally 100～140 DEG C), constantly in mixing kettle, add alkylene oxide monomer by alkylene oxide monomer charging aperture, it is sufficiently mixed under the linkage effect of the atomising device that the material returned with outer circulation is arranged in the mechanical agitation and outer circulation loop material charging aperture of mixing kettle, then passes to alkoxylation device；This stage keeps the temperature of mixing kettle lower than alkoxylation device 10～40 DEG C.
Ageing step: after being terminated by alkylene oxide monomer charging aperture addition alkylene oxide monomer, close alkylene oxide monomer charging aperture；The temperature keeping mixing kettle and alkoxylation device is in opening at reaction temperature, circulating pump and heat exchanger, keeps a period of time；
In the blowing stage: close the valve connecting alkoxylation device and circulating pump, close circulating pump and heat exchanger, open emptying device, discharging.
This utility model arranged mixing kettle before alkoxylation device, and initiator, catalyst, monomer and polyether intermediate are sufficiently mixed by described mixing kettle, and the alkoxylation device sending into next step carries out alkoxylation.Due to the mode adopting the atomising device of mechanical stirring device and still top outer circulation material charging aperture to combine, therefore the increase of polyethers viscosity is insensitive, the dispersion mixing of the relatively larger polyether intermediate of viscosity and epoxyalkane can be significantly improved, thus reaching good reaction effect in next step alkoxylation device.Preferably, described atomising device is atomizer well known in the art or Venturi nozzles, wherein atomizer is common in PRESS reactor, minimum drop can be atomized the liquid into into, Venturi nozzle is common in BUSS reactor, liquid can provide bigger kinetic energy so that gas-liquid is issued in strong kinetic energy condition and is sufficiently mixed.
This utility model is distributed many reacting pipes in alkoxylation device, the diameter of reacting pipe is significantly smaller than alkoxylation device, same alkoxylation device, reactant liquor flows through in the process of reacting pipe has higher draw ratio, reactant liquor is more abundant with the reaction of alkylene oxide monomer, thus having higher alkoxylation efficiency.
The reacting pipe that this utility model adopts, adopt the structure that large-diameter pipeline is alternately connected with small diameter pipeline, the reactant liquor of same flow flows through in the process of reacting pipe, owing to the diameter of pipeline is different, the flow velocity of fluid changes along with the change of reacting pipe diameter, so that reacting fluid keeps the state of complete turbulent flow in reacting pipe, same level section is close to complete mixing flow, there is higher Reynolds number, mass-and heat-transfer effect significantly improves, the mixing of reactant liquor and alkylene oxide monomer is more uniform, not only there is higher polymerization efficiency, and molecular weight control and molecular weight distribution be improved significantly.Owing to process fluid flow keeping complete turbulence state, especially for have the fluid of certain viscosity, there is higher mass-and heat-transfer efficiency equally.
The inner bag of described mixing kettle and internals material can be the materials such as rustless steel, enamel, the Acidity of Aikalinity reasonable selection according to initiator.
The mechanical stirring device of described mixing kettle can adopt one or more the combination in the structures such as plate and frame, anchor formula, paddle, screw, for the purpose of the mixing of materials effect reaching the best.
It is furthermore preferred that the length of reacting pipe is L in described alkoxylation device, the internal diameter of large-diameter pipeline is D, L/D is 50～500.The material of described alkoxylation device can be the one in the material such as rustless steel, enamel, the Acidity of Aikalinity reasonable selection according to reaction mass.
Preferably, the material in mixing kettle, with jacket structured, so can be heated or cool down by described mixing kettle, thus can be applied not only to liquid initiator, and is equally applicable for solid initiator.
This utility model can adopt DCS control, and material input and output material, pressure and temperature etc. are automatically controlled.
This utility model mixing of materials is fully, insensitive to the increase of polyethers viscosity, mass-and heat-transfer efficiency high, can be used for synthesizing the alkoxylation of unsaturated polyether；The selection of equipment is not significantly limited, it is possible to the difference according to the Acidity of Aikalinity of initiator, reasonably select the material of polyether reactant device；The amplification that according to actual production needs, can be carried out industrially scalable by non-geometric amplification method is produced, and alkoxylate efficiency etc. is unaffected.
Accompanying drawing explanation
Fig. 1 is the structural representation of the alkoxylation device that can be used for synthesizing unsaturated polyether；
Fig. 2 is the enlarged diagram of the partial reaction pipeline in Fig. 1；
Fig. 3 is the A-A cutaway view Amplified image of Fig. 1.
Detailed description of the invention
The present invention is described in detail below by example, these embodiments are merely illustrative, do not represent restriction the present invention the scope of application, in embodiment, device therefor, component, medicine or reagent all can be bought by usual channel, medicine or reagent be chemical pure and more than.Degree of unsaturation utilizes the method introduced in GB/T12008.7-92 to be measured, and molecular weight and molecualr weight distribution utilizes the GB/T27843-2011 method recommended to be measured.
Below in conjunction with drawings and the specific embodiments, this utility model made further description explanation.
As shown in Figures 1 to 3, a kind of alkoxylation device that can be used for unsaturated polyether synthesis, including the closed circuit that mixing kettle 4, alkoxylation device 6, circulating pump 10 and heat exchanger 11 order are connected in series.It is provided with mechanical stirring device 12 in described mixing kettle 4, top is provided with initiator/catalyst feeds 1 and the outer circulation loop material charging aperture 2 being connected with heat exchanger discharging opening, bottom is provided with alkylene oxide monomer charging aperture 3 and is connected to the mixing kettle discharging opening 19 at alkoxylation device top, is provided with the first valve 13 between mixing kettle discharging opening and alkoxylation device.It is provided with atomising device in described outer circulation loop material charging aperture 2.Axially disposed many reacting pipes 8 it are evenly distributed with in described alkoxylation device 6, the length of described reacting pipe 8 is L, alternately it is formed by connecting by large-diameter pipeline 15 and small diameter pipeline 16, internal diameter ratio (D/d) of large-diameter pipeline and small diameter pipeline is 1.2～3, and length ratio (L1/L2) is 1～10.Described alkoxylation device 6 be provided with between reacting pipe 8 space (in Fig. 1 shown in oblique dashed part) connect cooling water inlet 7, outlet 14, bottom is alkoxylation device discharging opening 9, described alkoxylation device discharging opening 9 is externally provided with the second valve 17, second valve 17 is connected with the 3rd valve the 18, the 4th valve 20 in parallel, wherein the 3rd valve 18 is connected to circulating pump 10, and the 4th valve is connected to discharging pipeline.
Following example adopt said apparatus to prepare unsaturated polyether.
Embodiment 1
Mixing kettle 4 and alkoxylation device 6 are stainless steel, wherein D/d=1.2, L1/L2=1, L/D=51.
Pretreatment stage: mixing kettle 4, alkoxylation device 6, circulating pump 10, heat exchanger 11 and pipeline dry in advance.
The stage of reaction: add initiator 1-propenol-3 200kg, catalyst KOH8kg from initiator/catalyst feeds 1 to mixing kettle 4, be then shut off initiator/catalyst feeds 1；Churned mechanically process is warmed up to about 60 DEG C, oxirane (hereinafter referred to as EO) 30kg is passed into from epoxyalkane charged monomer charging aperture 3 to mixing kettle 4, reaction to be polymerized starts, open the first valve 13 (alkoxylation device 6 is preheating to 100 DEG C in advance) connecting alkoxylation device 6, ON cycle pump 10 and heat exchanger 11；Keep mixing kettle 4 temperature at 90 DEG C, alkoxylation device 6 temperature is between 100～110 DEG C, reaction system pressure maintains 0.10～0.20MPa, constantly in mixing kettle 4, add EO by alkylene oxide monomer charging aperture 3, it is sufficiently mixed under the linkage effect of the atomizer that the material returned with outer circulation is arranged in the mechanical agitation 12 and outer circulation loop material charging aperture 2 of mixing kettle 4, passes into alkoxylation device 6.
Ageing step: add the accumulative 4200kg that reaches of EO, closedown alkylene oxide monomer charging aperture 3 by alkylene oxide monomer charging aperture 3；Keeping the temperature of mixing kettle 4 and alkoxylation device 6 between 100～110 DEG C, circulating pump 10 and heat exchanger 11 are in opening, retention time 2h.
In the blowing stage: close the 3rd valve 18 connecting alkoxylation device 6 and circulating pump 10, closing circulating pump 10 and heat exchanger 11, open emptying device, discharging, the material of releasing is shallow brown liquid.After tested: degree of unsaturation is 0.7812mol/kg, molecular weight is 1254, and molecular weight distribution is 1.02.
Embodiment 2
Mixing kettle 4 and alkoxylation device 6 are enamel material, wherein D/d=1.8, length ratio L1/L2=3, L/D=100.
Pretreatment stage: mixing kettle 4, alkoxylation device 6, circulating pump 10, heat exchanger 11 and pipeline dry in advance.
The stage of reaction: add initiator methallyl alcohol 100kg, catalyst n aH15kg (effective content 60%) from initiator/catalyst feeds 1 to mixing kettle 4, be then shut off initiator/catalyst feeds 1；Churned mechanically process is warmed up to about 70 DEG C, to mixing kettle 4, EO20kg is passed into from epoxyalkane charged monomer charging aperture 3, reaction to be polymerized starts, open the first valve 13 (alkoxylation device 6 is preheating to 105 DEG C in advance) connecting alkoxylation device 6, ON cycle pump 10 and heat exchanger 11；Keep mixing kettle 4 temperature at 100 DEG C, alkoxylation device 6 temperature is between 110～120 DEG C, reaction system pressure maintains 0.07～0.15MPa, constantly in mixing kettle 4, add EO by alkylene oxide monomer charging aperture 3, it is sufficiently mixed under the linkage effect of the Venturi nozzle that the material returned with outer circulation is arranged in the mechanical agitation 12 and outer circulation loop material charging aperture 2 of mixing kettle 4, passes into alkoxylation device 6.
Ageing step: add the accumulative 8000kg that reaches of EO, closedown alkylene oxide monomer charging aperture 3 by alkylene oxide monomer charging aperture 3；Keeping the temperature of mixing kettle 4 and alkoxylation device 6 between 100～110 DEG C, circulating pump 10 and heat exchanger 11 are in opening, retention time 1h.
In the blowing stage: close the 3rd valve 18 connecting alkoxylation device 6 and circulating pump 10, closing circulating pump 10 and heat exchanger 11, open emptying device, discharging, the material of releasing is shallow brown liquid.After tested: degree of unsaturation is 0.1698mol/kg, molecular weight is 5792, and molecular weight distribution is 1.01.
Embodiment 3
Mixing kettle 4 and alkoxylation device 6 are enamel material, wherein D/d=2.4, L1/L2=4, L/D=400.
Pretreatment stage: mixing kettle 4, alkoxylation device 6, circulating pump 10, heat exchanger 11 and pipeline dry in advance.
The stage of reaction: add initiator 3-methyl-3-butene-1-alcohol 400kg, catalyst CH from initiator/catalyst feeds 1 to mixing kettle 43ONa15kg, is then shut off initiator/catalyst feeds 1；Churned mechanically process is warmed up to about 80 DEG C, to mixing kettle 4, EO30kg is passed into from epoxyalkane charged monomer charging aperture 3, reaction to be polymerized starts, open the first valve 13 (alkoxylation device 6 is preheating to 110 DEG C in advance) connecting alkoxylation device 6, ON cycle pump 10 and heat exchanger 11；Keep mixing kettle 4 temperature at 100 DEG C, alkoxylation device 6 temperature is between 125～130 DEG C, reaction system pressure maintains 0.12～0.20MPa, constantly in mixing kettle 4, add EO by alkylene oxide monomer charging aperture 3, it is sufficiently mixed under the linkage effect of the atomizer that the material returned with outer circulation is arranged in the mechanical agitation 12 and outer circulation loop material charging aperture 2 of mixing kettle 4, passes into alkoxylation device 6.
Ageing step: add the accumulative 7700kg that reaches of EO, closedown alkylene oxide monomer charging aperture 3 by alkylene oxide monomer charging aperture 3；Keeping the temperature of mixing kettle 4 and alkoxylation device 6 between 120～125 DEG C, circulating pump 10 and heat exchanger 11 are in opening, retention time 1.5h.
In the blowing stage: close the 3rd valve 18 connecting alkoxylation device 6 and circulating pump 10, closing circulating pump 10 and heat exchanger 11, open emptying device, discharging, the material of releasing is shallow brown liquid.After tested: degree of unsaturation is 0.5713mol/kg, molecular weight is 1731, and molecular weight distribution is 1.02.
Embodiment 4
Mixing kettle 4 and alkoxylation device 6 are stainless steel, wherein D/d=2.8, L1/L2=5, L/D=490.
Pretreatment stage: mixing kettle 4, alkoxylation device 6, circulating pump 10, heat exchanger 11 and pipeline dry in advance.
The stage of reaction: add initiator hydroxy butyl vinyl ether 200kg, catalyst tBuOK5kg from initiator/catalyst feeds 1 to mixing kettle 4, be then shut off initiator/catalyst feeds 1；Churned mechanically process is warmed up to about 90 DEG C, to mixing kettle 4, EO30kg is passed into from epoxyalkane charged monomer charging aperture 3, reaction to be polymerized starts, open the first valve 13 (alkoxylation device 6 is preheating to 120 DEG C in advance) connecting alkoxylation device 6, ON cycle pump 10 and heat exchanger 11；Keep mixing kettle 4 temperature at 110 DEG C, alkoxylation device 6 temperature is between 125～135 DEG C, reaction system pressure maintains 0.20～0.30MPa, constantly in mixing kettle 4, add EO by alkylene oxide monomer charging aperture 3, it is sufficiently mixed under the linkage effect of the atomizer that the material returned with outer circulation is arranged in the mechanical agitation 12 and outer circulation loop material charging aperture 2 of mixing kettle 4, passes into alkoxylation device 6.
Ageing step: add the accumulative 2200kg that reaches of EO, closedown alkylene oxide monomer charging aperture 3 by alkylene oxide monomer charging aperture 3；Keeping the temperature of mixing kettle 4 and alkoxylation device 6 between 120～130 DEG C, circulating pump 10 and heat exchanger 11 are in opening, retention time 2h.
In the blowing stage: close the 3rd valve 18 connecting alkoxylation device 6 and circulating pump 10, closing circulating pump 10 and heat exchanger 11, open emptying device, discharging, the material of releasing is shallow brown liquid.After tested: degree of unsaturation is 0.7169mol/kg, molecular weight is 1378, and molecular weight distribution is 1.01.
Embodiment 5
Mixing kettle 4 and alkoxylation device 6 are stainless steel, wherein D/d=3, L1/L2=2, L/D=360.
Pretreatment stage: mixing kettle 4, alkoxylation device 6, circulating pump 10, heat exchanger 11 and pipeline dry in advance.
The stage of reaction: add the polyethers that initiator hydroxyethyl vinylethers, molecular weight are 200 (hydroxyethyl vinylethers is initiator from initiator/catalyst feeds 1 to mixing kettle 4, oxirane is monomer, little molecule polyethers through ring-opening polymerisation synthesis) it is total to 600kg (its middle-molecular-weihydroxyethyl is that the polyethers of 200 is as low-molecular-weight initiator), DMC catalysts DMC0.5kg, it is then shut off initiator/catalyst feeds 1；Churned mechanically process is warmed up to about 100 DEG C, expoxy propane (hereinafter referred to as PO) 10kg, EO50kg is passed into from epoxyalkane charged monomer charging aperture 3 to mixing kettle 4, reaction to be polymerized starts, open the first valve 13 (alkoxylation device 6 is preheating to 130 DEG C in advance) connecting alkoxylation device 6, ON cycle pump 10 and heat exchanger 11；Keep mixing kettle 4 temperature at 100 DEG C, alkoxylation device 6 temperature is between 130～140 DEG C, reaction system pressure maintains 0.30～0.40MPa, constantly in mixing kettle 4, add EO by alkylene oxide monomer charging aperture 3, it is sufficiently mixed under the linkage effect of the Venturi nozzle that the material returned with outer circulation is arranged in the mechanical agitation 12 and outer circulation loop material charging aperture 2 of mixing kettle 4, passes into alkoxylation device 6.
Ageing step: add the accumulative 5500kg that reaches of EO, closedown alkylene oxide monomer charging aperture 3 by alkylene oxide monomer charging aperture 3；Keeping the temperature of mixing kettle 4 and alkoxylation device 6 between 120～130 DEG C, circulating pump 10 and heat exchanger 11 are in opening, retention time 1h.
In the blowing stage: close the 3rd valve 18 connecting alkoxylation device 6 and circulating pump 10, closing circulating pump 10 and heat exchanger 11, open emptying device, discharging, the material of releasing is shallow brown liquid.After tested: degree of unsaturation is 0.4857mol/kg, molecular weight is 2050, and molecular weight distribution is 1.02.
Embodiment 6
Mixing kettle 4 and alkoxylation device 6 are stainless steel, wherein D/d=2.5, L1/L2=3, L/D=280.
Pretreatment stage: mixing kettle 4, alkoxylation device 6, circulating pump 10, heat exchanger 11 and pipeline dry in advance.
The stage of reaction: add the polyethers that initiator undecylenic alcohol, molecular weight are 400 (undecylenic alcohol is initiator from initiator/catalyst feeds 1 to mixing kettle 4, oxirane is monomer, little molecule polyethers through ring-opening polymerisation synthesis) it is total to 400kg (its middle-molecular-weihydroxyethyl is that the polyethers of 400 is as low-molecular-weight initiator), DMC catalysts DMC3.2kg, it is then shut off initiator/catalyst feed pipeline 1；Churned mechanically process is warmed up to about 120 DEG C, expoxy propane (hereinafter referred to as PO) 10kg, EO50kg is passed into from epoxyalkane charged monomer charging aperture 3 to mixing kettle 4, reaction to be polymerized starts, open the first valve 13 (alkoxylation device 6 is preheating to 120 DEG C in advance) connecting alkoxylation device 6, ON cycle pump 10 and heat exchanger 11；Keep mixing kettle 4 temperature at 110 DEG C, alkoxylation device 6 temperature is between 125～135 DEG C, reaction system pressure maintains 0.02～0.10MPa, constantly in mixing kettle 4, add EO by alkylene oxide monomer charging aperture 3, it is sufficiently mixed under the linkage effect of the atomizer that the material returned with outer circulation is arranged in the mechanical agitation 12 and outer circulation loop material charging aperture 2 of mixing kettle 4, passes into alkoxylation device 6.
Ageing step: add the accumulative 10000kg that reaches of EO, closedown alkylene oxide monomer charging aperture 3 by alkylene oxide monomer charging aperture 3；Keeping the temperature of mixing kettle 4 and alkoxylation device 6 between 120～125 DEG C, circulating pump 10 and heat exchanger 11 are in opening, retention time 1h.
In the blowing stage: close the 3rd valve 18 connecting alkoxylation device 6 and circulating pump 10, closing circulating pump 10 and heat exchanger 11, open emptying device, discharging, the material of releasing is shallow brown liquid.After tested: degree of unsaturation is 0.09593mol/kg, molecular weight is 9987, and molecular weight distribution is 1.02.
Above-described is only optimal way of the present utility model; it should be pointed out that, for the person of ordinary skill of the art, under the premise creating design without departing from this utility model; can also making some deformation and improvement, these also should be regarded as within protection domain of the present utility model.
Claims (5)
1. the alkoxylation device that can be used for unsaturated polyether synthesis, including alkoxylation device (6), the closed circuit that circulating pump (10) and heat exchanger (11) order are connected in series, it is characterized in that, also include the mixing kettle (4) being serially connected between heat exchanger (11) and alkoxylation device (6), mechanical stirring device (12) it is provided with in described mixing kettle (4), top is provided with initiator/catalyst feeds (1) and outer circulation loop material charging aperture (2) being connected with heat exchanger discharging opening, bottom is provided with alkylene oxide monomer charging aperture (3) and is connected to the mixing kettle discharging opening (19) at alkoxylation device (6) top, it is provided with atomising device in described outer circulation loop material charging aperture (2), axially disposed many reacting pipes (8) it are evenly distributed with in described alkoxylation device (6), described reacting pipe (8) is alternately formed by connecting by large-diameter pipeline (15) and small diameter pipeline (16), the internal diameter ratio of large-diameter pipeline (15) and small diameter pipeline (16) is 1.2～3, length ratio is 1～10.
2. can be used for the alkoxylation device of unsaturated polyether synthesis as claimed in claim 1, it is characterised in that the cooling water import and export that described alkoxylation device (6) is provided with between reacting pipe (8) that space connects.
3. can be used for the alkoxylation device of unsaturated polyether synthesis as claimed in claim 1, it is characterised in that the length of described reacting pipe (8) is L, and the internal diameter of large-diameter pipeline (15) is D, L/D is 50～500.
4. the alkoxylation device that can be used for unsaturated polyether synthesis as according to any one of claims 1 to 3, it is characterised in that described atomising device is atomizer or Venturi nozzles.
5. the alkoxylation device that can be used for unsaturated polyether synthesis as according to any one of claims 1 to 3, it is characterised in that described mixing kettle (4) is with jacket structured.
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| CN113600113A (en) * | 2021-08-02 | 2021-11-05 | 山东鸿瑞新材料科技有限公司 | System for improving molecular weight distribution of medium-molecular polyisobutylene |
| CN114409889A (en) * | 2021-12-13 | 2022-04-29 | 山东一诺威新材料有限公司 | Method for reducing tailing of high molecular weight part in polyether polyol synthesized by DMC catalysis |
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