CN105175592A - Low-molecular-weight vinyl polymer synthesizing method - Google Patents
Low-molecular-weight vinyl polymer synthesizing method Download PDFInfo
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Abstract
The invention provides a low-molecular-weight vinyl polymer synthesizing method. By means of the intermittent solution polymerization method, the molecular weight of a prepared low-molecular-weight polymer can be reduced from 3*105Da to 2*104Da. The mode that in the prior art, control over the molecular weight depends on a chain transfer agent is broken through, it is only needed that oxygen is introduced to participate in a reaction, and the more oxygen is introduced into a kettle, the lower the molecular weight of the obtained vinyl polymer is. Heat in the reaction kettle is stable as a whole due to existence of a solvent, the negative influence that the temperature is too high and accordingly the gel effect is caused does not occur, no chain transfer agent is introduced, the technical effect of lowering the molecular weight is achieved, and the problem of chain transfer agent residue does not exist. The monomer conversion rate is as high as 95%.
Description
Technical field
The present invention relates to a kind of synthetic method of low-molecular-weight ethylenic based polyalcohol, belong to technical field of polymer preparation.
Background technology
High molecular polymer is applied to all trades and professions in life already, such as methyl acrylic ester (Methylpropiolate) and esters of acrylic acid (acrylicester) are the conventional monomers manufacturing synthetic glass, sizing agent and plastics, and vinylbenzene (Styrene, St) the most important purposes of monomer is used to synthetic rubber and plastics, is used for producing styrene-butadiene rubber(SBR), polystyrene, styrofoam.Also for manufacturing the engineering plastics of multiple different purposes from other monomer copolymerizations, as obtained ABS resin with vinyl cyanide, butadiene copolymer, various household electrical appliance and industrial are widely used in.Vinylbenzene, mainly for the production of styrene series resin and styrene-butadiene rubber(SBR), is also one of raw material producing ion exchange resin and pharmaceuticals.In addition, vinylbenzene also can be used for the industries such as pharmacy, dyestuff, agricultural chemicals and ore dressing.Alpha-methyl styrene (Alpha-Methylstyrene, α-St) colourless liquid, there is pungent odour, be heated and be polymerized, inflammable.Can be used for producing coating, softening agent, be also used as solvent, organic synthesis.
Along with the application of vinyl monomer is more and more extensive, demand expands further.Not only more and more higher to the purity requirement of vinyl monomer raw material, the production line requirement that same reply is different, to synthesis gained to the molecular weight of polymkeric substance also have high requirement.The molecular weight of polymkeric substance has important impact to the physical and mechanical properties of product and processing characteristics, and molecular weight is always as the important performance indexes of polymkeric substance.The tensile strength of polymkeric substance raises along with the increase of molecular weight, when molecular weight is increased to a certain degree, is tending towards constant to the impact of physical strength.The reduction of molecular weight can reduce the entanglement between molecular chain, thus increases creep and stress relaxation.Polymkeric substance can be subject to the impact of ambient light, heat in the process used, and cause molecule chain break, what the thermal destruction of low-molecular-weight polymkeric substance was become is more prone to.This affects the hot workability of polymkeric substance equally.When molecular weight is larger, forcing machine can become difficulty in the process extruded, and in Bamboo-shaped, is difficult to obtain satisfied engineering sample.Coating used at present, tackiness agent etc. all need low-molecular(weight)polymer, so obtain suitable molecular weight or even low-molecular weight polymer is still the demand manufacturing industry at present.
The method of current production vinyl polymer is generally divided into mass polymerization and solution polymerization.(1) all can add initiator such as Diisopropyl azodicarboxylate (AIBN) in the course of the polymerization process and be used for initiated polymerization, and chain-transfer agent such as lauryl mercaptan (dodecylmercaptan) etc. is used as the molecular weight regulator of synthetic rubber, synthon, synthetic resins.This is the method be most widely used, but initiator and chain-transfer agent all can be residual to some extent in the polymer, affect the finished product purity.(2) be polymerized in water-isopropyl alcohol mixed solvent, hydrogen peroxide makees initiator, and this method needs the last handling process of loaded down with trivial details removing Virahol; (3) in the reactor that metal-salt and the tertiary amine aqueous solution are housed, add monomer and hydrogen peroxide solution respectively, until reacted, and contained metal ion causes environmental pollution.Therefore how to overcome above existing technological deficiency, the synthesis low-molecular-weight ethylenic based polyalcohol of polymerization process continuous prodution easy to control, easy, environment-protecting asepsis is the problem of necessary consideration.
Summary of the invention
In order to solve the problem of prior art, especially in order to solve the dependency of adjustment to chain-transfer agent of polymericular weight, being polymerized to basis with batch solution, the invention provides a kind of synthetic method of low-molecular-weight ethylenic based polyalcohol.
the invention provides a kind of synthetic method of low-molecular-weight ethylenic based polyalcohol, step and condition as follows:
(1) weight of raw material is:
Vinyl monomer 50-90 part;
Solvent toluene is 10-50 part, the two and be 100 weight parts;
Initiator di-t-butyl peroxide 0.01-0.1 part;
the weight of preferred feedstock is:
Vinyl monomer 60-80 part;
Solvent toluene is 20-40 part; The two and be 100 weight parts;
Initiator di-t-butyl peroxide 0.05 part;
more preferably weight is:
Vinyl monomer 70 parts;
Solvent toluene is 30 parts;
Initiator di-t-butyl peroxide 0.05 part;
Described vinyl monomer is methyl methacrylate, butyl methacrylate, methyl acrylate, butyl acrylate, vinylbenzene or alpha-methyl styrene;
(2) batch solution polymerization is adopted to be polymerized:
According to weight, raw material is mixed, adopt meter Dun Luo diaphragm type charge pump, add in reactor, stir, stirring velocity 170r/min, in reactor, pass into nitrogen purge, air displacement in still is gone out, is heated to 130-150 DEG C, from heat up start, the purity passing into 0.1-0.3Mpa in batch reactor is the high purity oxygen gas of 99.995%, reaction times 5-6 hour, blowing, obtains target product.
beneficial effect:the synthetic method of a kind of low-molecular-weight ethylenic based polyalcohol of the present invention.Adopt batch solution polymerization, the molecular weight of the low-molecular weight polymer of preparation can from 3 × 10
5da is reduced to 2 × 10
4da.The present invention breaches in the past that dependency chain transfer agent is to carry out the control methods of molecular weight, and only need pass into oxygen and participate in reacting, the amount of oxygen passed in still is higher, and the molecular weight of the vinyl polymer obtained is lower.Methyl methacrylate number-average molecular weight (Da) is 28,000; The number-average molecular weight (Da) of methyl acrylate polymer is 27,000; The number-average molecular weight (Da) of butyl acrylate thing is 30,000; The number-average molecular weight (Da) of styrene polymer is 25,000; The number-average molecular weight (Da) of alpha-methyl styrene polymer is 31,000.Because of the existence of solvent, heat in reactor is steadily overall, there will not be that temperature is too high causes the negative impacts such as gel effect, does not introduce any chain-transfer agent, reaches and fall low-molecular-weight technique effect, there is not the problem that chain-transfer agent is residual.Monomer conversion is up to 95%.
Accompanying drawing explanation
Fig. 1 is the polymethylmethacrylate time conversion rate curve that embodiment 3 is synthesized.
Fig. 2 is the polymethyl acrylate time conversion rate curve that embodiment 7 is synthesized.
Fig. 3 is the polystyrene time conversion rate curve that embodiment 9 is synthesized.
Embodiment
embodiment 1a kind of synthetic method of low-molecular-weight ethylenic based polyalcohol.Described vinyl monomer is methyl methacrylate.
(1) weight is:
Methyl methacrylate 70 parts;
Solvent toluene is 30 parts;
Initiator di-t-butyl peroxide 0.05 part;
(2) batch solution polymerization: get main monomer methyl methacrylate 70 parts, solvent toluene is 30 parts, initiator di-t-butyl peroxide 0.05 part; I.e. methyl methacrylate 700 grams, toluene 300 grams, after di-t-butyl peroxide 0.35 gram mixes, meter Dun Luo diaphragm type charge pump is adopted to add in reactor, stir, stirring velocity 170r/min, passes into nitrogen and purges in reactor, air displacement in still is gone out, adopt oil bath carry out being heated to 130 DEG C, from heat up in reactor, pass into the high purity oxygen gas that 0.1Mpa purity is 99.995%, 6 hours reaction times, blowing, obtains target product.
In accordance with the following methods the number-average molecular weight of target product is tested:
Gel permeation chromatography: AllianceGPCV2000 type gel chromatograph, using tetrahydrofuran (THF) as moving phase, monodispersed polystyrene is that standard specimen is used as universal calibration.Solvent flow rate is 1mL/min, and probe temperature is 35 ° of C.Test result is as shown in table 1.
embodiment 2a kind of synthetic method of low-molecular-weight ethylenic based polyalcohol.Described vinyl monomer is methyl methacrylate.
(1) weight is:
Methyl methacrylate 70 parts;
Solvent toluene is 30 parts;
Initiator di-t-butyl peroxide 0.05 part;
(2) batch solution polymerization:
Batch solution is polymerized: get main monomer methyl methacrylate 70 parts, solvent toluene 30 parts, di-t-butyl peroxide 0.05 part, i.e. methyl methacrylate 700 grams, toluene 300 grams, di-t-butyl peroxide 0.35 gram.After monomer, solvent are mixed with initiator, meter Dun Luo diaphragm type charge pump is adopted to add in the reactor of 2 liters, setting stirring velocity 170r/min, the mode of nitrogen purging is adopted the air displacement in still to be gone out, oil bath is adopted to carry out being heated to 130 DEG C, from heat up in still, pass into the high purity oxygen gas that 0.2Mpa purity is 99.995%, react 6 hours, obtain subject polymer.
Test is as embodiment 1, and result is as shown in table 1.
embodiment 3a kind of synthetic method of low-molecular-weight ethylenic based polyalcohol.Described vinyl monomer is methyl methacrylate.
(1) weight is:
Methyl methacrylate 70 parts;
Solvent toluene is 30 parts;
Initiator di-t-butyl peroxide 0.05 part;
(2) batch solution polymerization: get main monomer methyl methacrylate 70 parts, solvent toluene 30 parts, di-t-butyl peroxide 0.05 part, i.e. methyl methacrylate 700 grams, toluene 300 grams, di-t-butyl peroxide 0.35 gram.After monomer, solvent are mixed with initiator, meter Dun Luo diaphragm type charge pump is adopted to add in the reactor of 2 liters, setting stirring velocity 170r/min, the mode of nitrogen purging is adopted the air displacement in still to be gone out, oil bath is adopted to carry out being heated to 130 DEG C, from heat up in still, pass into the high purity oxygen gas that 0.3Mpa purity is 99.995%, react 5 hours, obtain subject polymer.Measured polymer conversion monitoring result as shown in Figure 1, that represent is polymethyl acrylate time conversion rate curve figure, through the Real-Time Monitoring polymer conversion change of 5 hours, the solution polymerization process that oxygen participates in can allow monomer, and transformation efficiency was up to 95.3% at short notice, and rate of polymerization is very fast.
Test is as embodiment 1, and result is as shown in table 1.
embodiment 4a kind of synthetic method of low-molecular-weight ethylenic based polyalcohol.Described vinyl monomer is methyl methacrylate.
(1) weight is:
Methyl methacrylate 70 parts;
Solvent toluene is 30 parts;
Initiator di-t-butyl peroxide 0.035 part;
(2) batch solution polymerization: get main monomer methyl methacrylate 70 parts, solvent toluene 30 parts, di-t-butyl peroxide 0.035 part, i.e. methyl methacrylate 700 grams, toluene 300 grams, di-t-butyl peroxide 0.245 gram.After monomer, solvent are mixed with initiator, meter Dun Luo diaphragm type charge pump is adopted to add in the reactor of 2 liters, setting stirring velocity 170r/min, the mode of nitrogen purging is adopted the air displacement in still to be gone out, oil bath is adopted to carry out being heated to 140 DEG C, from heat up in still, pass into the high purity oxygen gas that 0.3Mpa purity is 99.995%, react 5 hours, obtain subject polymer.
Test is as embodiment 1, and result is as shown in table 1.
embodiment 5a kind of synthetic method of low-molecular-weight ethylenic based polyalcohol.Described vinyl monomer is methyl methacrylate.
(1) weight is:
Methyl methacrylate 70 parts;
Solvent toluene is 30 parts;
Initiator di-t-butyl peroxide 0.035 part;
(2) batch solution polymerization: get main monomer methyl methacrylate 70 parts, solvent toluene 30 parts, di-t-butyl peroxide 0.035 part, i.e. methyl methacrylate 700 grams, toluene 300 grams, di-t-butyl peroxide 0.245 gram.After monomer, solvent are mixed with initiator, meter Dun Luo diaphragm type charge pump is adopted to add in the reactor of 2 liters, setting stirring velocity 170r/min, the mode of nitrogen purging is adopted the air displacement in still to be gone out, oil bath is adopted to carry out being heated to 150 DEG C, from heat up in still, pass into the high purity oxygen gas that 0.3Mpa purity is 99.995%, react 5 hours, obtain subject polymer.
Test is as embodiment 1, and result is as shown in table 1.
embodiment 6a kind of synthetic method of low-molecular-weight ethylenic based polyalcohol.Described vinyl monomer is butyl methacrylate.
(1) weight is:
Butyl methacrylate 60 parts;
Solvent toluene is 40 parts;
Initiator di-t-butyl peroxide 0.01 part;
(2) batch solution polymerization:
Get main monomer butyl methacrylate 60 parts, solvent toluene 40 parts, di-t-butyl peroxide 0.01 part, i.e. butyl methacrylate 600 grams, toluene 400 grams, di-t-butyl peroxide 0.06 gram.After monomer, solvent are mixed with initiator, meter Dun Luo diaphragm type charge pump is adopted to add in the reactor of 2 liters, setting stirring velocity 170r/min, the mode of nitrogen purging is adopted the air displacement in still to be gone out, oil bath is adopted to carry out being heated to 130 DEG C, from heat up and pass into into 0.3Mpa purity in still to be the high purity oxygen gas of 99.995%, to react after 6 hours, obtain subject polymer.
Test is as embodiment 1, and result is as shown in table 1.
embodiment 7a kind of synthetic method of low-molecular-weight ethylenic based polyalcohol.Described vinyl monomer is methyl acrylate.
(1) weight is:
Methyl acrylate 50 parts;
Solvent toluene is 50 parts;
Initiator di-t-butyl peroxide 0.1 part;
(2) batch solution polymerization:
Get main monomer methyl acrylate 50 parts, solvent toluene 50 parts, di-t-butyl peroxide 0.1 part, i.e. methyl acrylate 500 grams, toluene 500 grams, di-t-butyl peroxide 0.5 gram.After monomer, solvent are mixed with initiator, meter Dun Luo diaphragm type charge pump is adopted to add in the reactor of 2 liters, setting stirring velocity 170r/min, the mode of nitrogen purging is adopted the air displacement in still to be gone out, oil bath is adopted to carry out being heated to 130 DEG C, from heat up in still, pass into the high purity oxygen gas that 0.3Mpa purity is 99.995%, react 6 hours, obtain subject polymer.
Measured polymer conversion monitoring result as shown in Figure 2, that represent is polymethyl acrylate time conversion rate curve figure, through the Real-Time Monitoring polymer conversion change of 6 hours, the solution polymerization process that oxygen participates in can allow monomer, and transformation efficiency was up to 94.6% at short notice, and rate of polymerization is very fast.
Test is as embodiment 1, and result is as shown in table 1.
embodiment 8a kind of synthetic method of low-molecular-weight ethylenic based polyalcohol.Described vinyl monomer is butyl acrylate.
(1) weight is:
Butyl acrylate 80 parts;
Solvent toluene is 20 parts;
Initiator di-t-butyl peroxide 0.05 part;
(2) batch solution polymerization:
Get main monomer butyl acrylate 80 parts, solvent toluene 20 parts, di-t-butyl peroxide 0.05 part, i.e. butyl acrylate 800 grams, toluene 200 grams, di-t-butyl peroxide 0.4 gram.After monomer, solvent are mixed with initiator, meter Dun Luo diaphragm type charge pump is adopted to add in the reactor of 2 liters, setting stirring velocity 170r/min, the mode of nitrogen purging is adopted the air displacement in still to be gone out, oil bath is adopted to carry out being heated to 130 DEG C, from heat up in still, pass into the high purity oxygen gas that 0.3Mpa purity is 99.995%, react 6 hours, obtain subject polymer.
Testing standard is as embodiment 1, and result is as shown in table 1.
embodiment 9a kind of synthetic method of low-molecular-weight ethylenic based polyalcohol.Described vinyl monomer is vinylbenzene.
(1) weight is:
Vinylbenzene 90 parts;
Solvent toluene is 10 parts;
Initiator di-t-butyl peroxide 0.045 part;
(2) batch solution polymerization:
Get main monomer vinylbenzene 90 parts, solvent toluene 10 parts, di-t-butyl peroxide 0.045 part, i.e. vinylbenzene 900 grams, toluene 100 grams, di-t-butyl peroxide 0.405 gram.After monomer, solvent are mixed with initiator, meter Dun Luo diaphragm type charge pump is adopted to add in the reactor of 2 liters, setting stirring velocity 170r/min, the mode of nitrogen purging is adopted the air displacement in still to be gone out, oil bath is adopted to carry out being heated to 130 DEG C, from heat up in still, pass into the high purity oxygen gas that 0.3Mpa purity is 99.995%, react 6 hours, obtain subject polymer.
Measured polymer conversion monitoring result as shown in Figure 3, that represent is polystyrene time conversion rate curve figure, through the Real-Time Monitoring polymer conversion change of 6 hours, the solution polymerization process that oxygen participates in can allow monomer, and transformation efficiency was up to 95.1% at short notice, and rate of polymerization is very fast.
Test is as embodiment 1, and result is as shown in table 1.
embodiment 10a kind of synthetic method of low-molecular-weight ethylenic based polyalcohol.Described vinyl monomer is alpha-methyl styrene.
(1) weight is:
Alpha-methyl styrene 70 parts;
Solvent toluene is 30 parts;
Initiator di-t-butyl peroxide 0.035 part;
(2) batch solution polymerization:
Get main monomer alpha-methyl styrene 70 parts, solvent toluene 30 parts, di-t-butyl peroxide 0.035 part, i.e. alpha-methyl styrene 700 grams, toluene 300 grams, di-t-butyl peroxide 0.245 gram.After monomer, solvent are mixed with initiator, meter Dun Luo diaphragm type charge pump is adopted to add in the reactor of 2 liters, setting stirring velocity 170r/min, the mode of nitrogen purging is adopted the air displacement in still to be gone out, oil bath is adopted to carry out being heated to 130 DEG C, from heat up in still, pass into the high purity oxygen gas that 0.3Mpa purity is 99.995%, react 6 hours, obtain subject polymer.
Test is as embodiment 1, and result is as shown in table 1.
Table 1 low-molecular-weight ethylenic based polyalcohol number-average molecular weight test result
Claims (8)
1. a synthetic method for low-molecular-weight ethylenic based polyalcohol, is characterized in that, step and condition as follows:
(1) weight of raw material is:
Vinyl monomer 50-90 part;
Solvent toluene is 10-50 part, the two and be 100 weight parts;
Initiator di-t-butyl peroxide 0.01-0.1 part;
Described vinyl monomer is methyl methacrylate, butyl methacrylate, methyl acrylate, butyl acrylate, vinylbenzene or alpha-methyl styrene;
(2) batch solution polymerization is adopted to be polymerized:
According to weight, raw material is mixed, adopt meter Dun Luo diaphragm type charge pump, add in reactor, stir, stirring velocity 170r/min, in reactor, pass into nitrogen purge, air displacement in still is gone out, is heated to 130-150 DEG C, from heat up start, the purity passing into 0.1-0.3Mpa in batch reactor is the high purity oxygen gas of 99.995%, reaction times 5-6 hour, blowing, obtains target product.
2. the synthetic method of a kind of low-molecular-weight ethylenic based polyalcohol as claimed in claim 1, is characterized in that, the weight of raw material is:
Vinyl monomer 60-80 part;
Solvent toluene is 20-40 part; The two and be 100 weight parts;
Initiator di-t-butyl peroxide 0.05 part.
3. the synthetic method of a kind of low-molecular-weight ethylenic based polyalcohol as claimed in claim 1, is characterized in that, the weight of raw material is:
Vinyl monomer 70 parts;
Solvent toluene is 30 parts;
Initiator di-t-butyl peroxide 0.05 part.
4. the synthetic method of a kind of low-molecular-weight ethylenic based polyalcohol as claimed in claim 1, is characterized in that, step and condition as follows: described vinyl monomer is methyl methacrylate;
(1) weight is:
Methyl methacrylate 70 parts;
Solvent toluene is 30 parts;
Initiator di-t-butyl peroxide 0.05 part;
(2) batch solution polymerization: by proportioning, after monomer, solvent are mixed with initiator, meter Dun Luo diaphragm type charge pump is adopted to add in reactor, setting stirring velocity 170r/min, adopt the mode of nitrogen purging the air displacement in still to be gone out, adopt oil bath to carry out being heated to 130 DEG C, from heat up in still, pass into the high purity oxygen gas that 0.3Mpa purity is 99.995%, react 5 hours, obtain subject polymer.
5. the synthetic method of a kind of low-molecular-weight ethylenic based polyalcohol as claimed in claim 1, is characterized in that, step and condition as follows: described vinyl monomer is methyl methacrylate;
(1) weight is:
Methyl methacrylate 70 parts;
Solvent toluene is 30 parts;
Initiator di-t-butyl peroxide 0.035 part;
(2) batch solution polymerization: by proportioning, after monomer, solvent are mixed with initiator, meter Dun Luo diaphragm type charge pump is adopted to add in reactor, setting stirring velocity 170r/min, adopt the mode of nitrogen purging the air displacement in still to be gone out, adopt oil bath to carry out being heated to 150 DEG C, from heat up in still, pass into the high purity oxygen gas that 0.3Mpa purity is 99.995%, react 5 hours, obtain subject polymer.
6. the synthetic method of a kind of low-molecular-weight ethylenic based polyalcohol as claimed in claim 1, is characterized in that, step and condition as follows: described vinyl monomer is methyl acrylate;
(1) weight is:
Methyl acrylate 50 parts;
Solvent toluene is 50 parts;
Initiator di-t-butyl peroxide 0.1 part;
(2) batch solution polymerization: by proportioning, after monomer, solvent are mixed with initiator, meter Dun Luo diaphragm type charge pump is adopted to add in reactor, setting stirring velocity 170r/min, adopt the mode of nitrogen purging the air displacement in still to be gone out, adopt oil bath to carry out being heated to 130 DEG C, from heat up in still, pass into the high purity oxygen gas that 0.3Mpa purity is 99.995%, react 6 hours, obtain subject polymer.
7. the synthetic method of a kind of low-molecular-weight ethylenic based polyalcohol as claimed in claim 1, is characterized in that, step and condition as follows: described vinyl monomer is butyl acrylate;
(1) weight is:
Butyl acrylate 80 parts;
Solvent toluene is 20 parts;
Initiator di-t-butyl peroxide 0.05 part;
(2) batch solution polymerization: by proportioning, after monomer, solvent are mixed with initiator, meter Dun Luo diaphragm type charge pump is adopted to add in the reactor of 2 liters, setting stirring velocity 170r/min, adopt the mode of nitrogen purging the air displacement in still to be gone out, adopt oil bath to carry out being heated to 130 DEG C, from heat up in still, pass into the high purity oxygen gas that 0.3Mpa purity is 99.995%, react 6 hours, obtain subject polymer.
8. the synthetic method of a kind of low-molecular-weight ethylenic based polyalcohol as claimed in claim 1, is characterized in that, step and condition as follows: described vinyl monomer is vinylbenzene;
(1) weight is:
Vinylbenzene 90 parts;
Solvent toluene is 10 parts;
Initiator di-t-butyl peroxide 0.045 part;
(2) batch solution polymerization: by proportioning, after monomer, solvent are mixed with initiator, meter Dun Luo diaphragm type charge pump is adopted to add in reactor, setting stirring velocity 170r/min, adopt the mode of nitrogen purging the air displacement in still to be gone out, adopt oil bath to carry out being heated to 130 DEG C, from heat up in still, pass into the high purity oxygen gas that 0.3Mpa purity is 99.995%, react 6 hours, obtain subject polymer.
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| WO2023006322A1 (en) * | 2021-07-29 | 2023-02-02 | Evonik Operations Gmbh | Process for preparing low molecular weight polyacrylates and products thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080058482A1 (en) * | 2006-08-29 | 2008-03-06 | 3M Innovative Properties Company | Continuous process polymerization of (meth)acrylate copolymers |
| CN103261241A (en) * | 2010-12-22 | 2013-08-21 | 巴塞尔聚烯烃股份有限公司 | Process for monitoring the polymerization of ethylene or ethylene and comonomers in tubular-eactor at high-pressures |
-
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080058482A1 (en) * | 2006-08-29 | 2008-03-06 | 3M Innovative Properties Company | Continuous process polymerization of (meth)acrylate copolymers |
| CN103261241A (en) * | 2010-12-22 | 2013-08-21 | 巴塞尔聚烯烃股份有限公司 | Process for monitoring the polymerization of ethylene or ethylene and comonomers in tubular-eactor at high-pressures |
Non-Patent Citations (1)
| Title |
|---|
| T. MUKUNDAN ET AL.: ""Poly(vinylnaphtha1ene peroxide)s: Syntheses, Characterization, and Thermal Reactivity"", 《MACROMOLECULES》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023006322A1 (en) * | 2021-07-29 | 2023-02-02 | Evonik Operations Gmbh | Process for preparing low molecular weight polyacrylates and products thereof |
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