CN109748986A - The method that low-molecular-weight polystyrene is prepared by styrene using microreactor - Google Patents
The method that low-molecular-weight polystyrene is prepared by styrene using microreactor Download PDFInfo
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Abstract
A method of low-molecular-weight polystyrene being prepared by styrene using microreactor, by the way that monomer styrene and initiator toluene solution are inputted from two different arrival ends of T-shaped micro-mixer respectively, enter after mixing and carries out polymerization reaction in reacting pipe, after the purified drying of product, powdered polystyrene is obtained；The present invention makes to shorten within 30min the time required to sufficiently reacting, and reaction temperature is 60~140 DEG C, and product dispersion index is 1.1~2.0, and number-average molecular weight is adjustable in 1000~10000 ranges, has good promotion prospect.
Description
Technical field
It is specifically a kind of to utilize microreactor the present invention relates to the technology of a kind of chemical process and polymerization reaction field
The method that low-molecular-weight polystyrene is prepared by styrene.
Background technique
The synthesis of polystyrene (PS) has had more than 70 years since nineteen thirty-five realizes industrialized production with mass polymerization
Developing history.Since it has preferable rigid, transparent, water-fast, corrosion resistance, electrical insulating property and low hygroscopicity, and valence
The features such as lattice are cheap, easily molded processing and coloring is widely used in the neck such as instrument and meter component, decoration, packaging and articles for daily use
Domain.In the production process of industrialized polystyrene, first styrene is mixed with toluene or ethylbenzene, the shape in autoclave blender
At homogeneous phase solution；Then initiator is dissolved in toluene or ethylbenzene solution, is added drop-wise in styrene solution with certain speed, and
Stirring, then pass through heating initiated polymerization.Since styrene polymerization reaction heat is 71.72kJ/mol, and as polymerization is anti-
The progress answered, the viscosity of Polymer Solution gradually increase, and traditional tank reactor is for the Polymer Solution with high viscosity
Mixing, heat transfer property are poor, are easy to cause monomer concentration to be unevenly distributed during the reaction, and local temperature is excessively high, occur certainly
Dynamic acceleration effect even implode, it is bad to eventually lead to product batches stability.Meanwhile the intermittent reaction operation cycle is long, production capacity is low,
Energy consumption is high.
Summary of the invention
The defects of present invention is cumbersome for prior art operation mode, and the reaction time is long and lot stability is poor, proposes
A method of low-molecular-weight polystyrene being prepared by styrene using microreactor, the reaction time foreshortens to 5~30min, single
90% or more transformation rate, molecular weight 1000-10000, molecular weight distribution 1.1-2.0, solvent and residual monomer are recyclable
It uses.
The present invention is achieved by the following technical solutions:
The present invention from the two of T-shaped micro-mixer differences by entering monomer styrene and initiator toluene solution respectively
The input of mouth end, enters after mixing and carries out polymerization reaction in reacting pipe, after the purified drying of product, obtain powdered polyphenyl second
Alkene.
The monomer solution concentration is 0.5~5mol/L, and the feeding temperature of monomer solution is 10~50 DEG C.
Preferably, polymerization reaction is carried out in reacting pipe, passes through constent temperature heater or the control control of other temperature conditioning units
Polymeric reaction temperature is 60~140 DEG C, and the polystyrene solution obtained after polymerization reaction enters collecting tank from reaction pipeline outflow.
The initiator is azodiisobutyronitrile (AIBN), dibenzoyl peroxide (BPO) or perbenzoic acid uncle
One of butyl ester (TBPB) or more；The dosage of solvent toluene is 0.1~5.0 times of volume of styrene, and initiator amount is
The 1~10% of monomer mass, the toluene solution feeding temperature dissolved with initiator are 10~50 DEG C.
Preferably, the polystyrene solution obtained after polymerization reaction is purified using alcoholic solvent, and the polystyrene after purification is
White stringy solids obtain powdery product polystyrene after drying.The raffinate of purification polystyrene obtains after being evaporated under reduced pressure
Alcoholic solvent be circularly used for the purification of polystyrene.
The solvent of the purification polystyrene is methanol and/or ethyl alcohol.
Technical effect
Compared with prior art, microreactor of the present invention can effectively strengthen the mixed process of monomer and initiator, strengthen
Heat transfer process removes polymerization reaction heat in time, the accurate reaction temperature controlled inside reacting pipe, and using continuously flowing
Production model solves the problems, such as the lot stability of product.Result of study shows that the device can be in 60~140 DEG C of temperature model
Enclose the interior styrene solution polymerization for realizing serialization.
Detailed description of the invention
Fig. 1 is microreactor apparatus structure schematic diagram；
In figure: 1 styrene solution storage tank, the toluene solution storage tank of 2 initiators, 3 alcoholic solvent storage tanks, 4 advection pumps, 5
Advection pump, 6 advection pumps, 7T font micro-mixer, 8 reacting pipes, 9 sample collection tanks；
Specific embodiment
Embodiment 1
As shown in Figure 1, the present embodiment is accomplished by the following way:
1) styrene solution and initiator solution are separately stored in storage tank 1 and 2, from advection pump 4 and 5 convey into
Enter micro-mixer 7, two kinds of solution are mixed in micro-mixer；
2) polymerization reaction is carried out in reacting pipe 8, controlling reaction temperature by oil bath is 60~140 DEG C, reacting pipe
The solution storage that exit obtains is in collecting tank 9.
3) alcoholic solvent in storage tank 3 is delivered in collecting tank 9 through advection pump 6, and the polystyrene after purification is white
Stringy solids obtain powdered polystyrene after drying.
The T-shaped micro-mixer that the present embodiment is 0.5mm using internal diameter, reacting pipe internal diameter are 0.5mm.Solvent toluene
Volumetric usage is 2 times of styrene, and initiator B PO mass dosage is the 5% of styrene.Temperature in reacting pipe is 100 DEG C,
Reaction flow quantity is 1.0ml/min, reaction time 15min.The number-average molecular weight Mn of product is 4876, and molecular weight distributing index is
1.35, monomer conversion 95.54%.
Embodiment 2
The volumetric usage of the present embodiment solvent toluene is 5 times of styrene, and other conditions are same as Example 1.This implementation
The number-average molecular weight Mn of example products therefrom is 3682, molecular weight distributing index 1.55, conversion ratio 91.45%.
Embodiment 3
The present embodiment, reaction time 30min, other conditions are same as Example 1.The number of the present embodiment products therefrom is equal
Molecular weight Mn is 4668, molecular weight distributing index 1.41, conversion ratio 98.70%.
Embodiment 4
The present embodiment initiator is AIBN, and other conditions are same as Example 1.The equal molecule of the number of the present embodiment products therefrom
Measuring Mn is 3570, molecular weight distributing index 1.65, conversion ratio 90.2%.
Embodiment 5
The present embodiment initiator B PO dosage is the 1% of styrene quality, and other conditions are same as Example 1.The present embodiment
The number-average molecular weight Mn of products therefrom is 9006, molecular weight distributing index 1.63, conversion ratio 93.67%.
Embodiment 6
The internal diameter for the capillary reaction pipeline that the present embodiment uses is 3mm, and other conditions are same as Example 1.This implementation
The number-average molecular weight Mn of example products therefrom is 5208, molecular weight distributing index 1.86, conversion ratio 90.51%.
Embodiment 7
The present embodiment reaction temperature is 140 DEG C, and other conditions are same as Example 1.The number of the present embodiment products therefrom is equal
Molecular weight Mn is 2408, molecular weight distributing index 1.86, conversion ratio 99.02%.
Above-mentioned specific implementation can by those skilled in the art under the premise of without departing substantially from the principle of the invention and objective with difference
Mode carry out local directed complete set to it, protection scope of the present invention is subject to claims and not by above-mentioned specific implementation institute
Limit, each implementation within its scope is by the constraint of the present invention.
Claims (9)
1. a kind of method for preparing low-molecular-weight polystyrene by styrene using microreactor, which is characterized in that by will be single
Body styrene and initiator toluene solution enter anti-respectively from two different arrival end inputs of T-shaped micro-mixer after mixing
Progress polymerization reaction in pipeline is answered to obtain powdered polystyrene after the purified drying of product.
2. method according to claim 1, characterized in that the internal diameter of the T-shaped micro-mixer is 0.2mm~6mm.
3. method according to claim 1, characterized in that the volumetric usage of the solvent toluene is the 0.1~5.0 of styrene
Times, the feeding temperature of monomer solution is 10~50 DEG C.
4. method according to claim 1, characterized in that the initiator be azodiisobutyronitrile, dibenzoyl peroxide or
One or more of peroxidized t-butyl perbenzoate；Initiator quality dosage is the 1~10% of monomer, the toluene solution of initiator
Feeding temperature is 10~50 DEG C.
5. method according to claim 1, characterized in that controlling control polymeric reaction temperature by constent temperature heater is 60~140
DEG C, the polystyrene solution obtained after polymerization reaction enters collecting tank from reaction pipeline outflow.
6. according to claim 1 or 5 methods, characterized in that the reacting pipe is capillary, and internal diameter is 0.25~6mm, long
Degree is 3~30m, and reaction flow velocity is 0.5~3mL/min, 5~30min of reaction solution residence time in reacting pipe.
7. according to claim 1 or 5 methods, characterized in that utilize 2-100 reacting pipe, each reacting pipe front end connects
Distributor is operated using the mode of arranged in parallel, and reaction flow velocity is 0.5~3mL/min, reaction in each reacting pipe
5~30min of liquid residence time.
8. method according to claim 1, characterized in that the polystyrene solution obtained after polymerization reaction is purified using alcoholic solvent,
Polystyrene after purification is white stringy solids, and powdery product polystyrene is obtained after drying；Purify the residual of polystyrene
The alcoholic solvent that liquid obtains after being evaporated under reduced pressure then recycles the purification for polystyrene.
9. method according to claim 1, characterized in that the solvent of the purification polystyrene is methanol and/or ethyl alcohol.
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| CN201711075397.0A CN109748986A (en) | 2017-11-06 | 2017-11-06 | The method that low-molecular-weight polystyrene is prepared by styrene using microreactor |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111330521A (en) * | 2020-03-06 | 2020-06-26 | 山东旭锐新材有限公司 | Styrene polymerization micro-reaction device and micro-reaction method |
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2017
- 2017-11-06 CN CN201711075397.0A patent/CN109748986A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111330521A (en) * | 2020-03-06 | 2020-06-26 | 山东旭锐新材有限公司 | Styrene polymerization micro-reaction device and micro-reaction method |
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Application publication date: 20190514 |