18 results about "Living polymerization" patented technology

The invention provides a flexible switching production method and equipment for low cis-polybutadiene rubber (LCBR), solution polymerized styrene-butadiene rubber (SSBR) and hydroxyl-terminated liquid polybutadiene rubber (HTPB), the flexible switching production equipment comprises an initiator production device and a polymerization unit, and the flexible switching production method comprises the following steps: mixing cyclohexane and n-hexane according to a volume ratio of 6.5: 3.5-7: 3, adding an initiator, and stirring to obtain a mixture; forming a mixed solvent; the method comprises the following steps: adding a monomer, an active agent, an initiator and a mixed solvent into a polymerization kettle 31 of a polymerization unit, and carrying out polymerization reaction to obtain a low-cis-polybutadiene, solution polymerized styrene-butadiene or hydroxyl-terminated liquid polybutadiene rubber solution; a novel protection initiator tert-butyl dimethyl siloxy propyl sodium is designed, and hydroxyl-terminated liquid polybutadiene rubber with a controllable structure is prepared through anionic living polymerization. According to the process, shutdown for kettle cleaning is not needed, the low cis-polybutadiene, the solution polymerized styrene-butadiene and the hydroxyl-terminated liquid polybutadiene rubber can be produced on the same polymerization device in a flexible switching manner, and the overall production efficiency is improved.

The invention discloses an alkyl magnesium reagent-based active anionic polymerization initiation system and a polymerization method, and belongs to the technical field of polymer synthesis. A novel initiation system based on an alkyl magnesium reagent is developed, controllable anionic polymerization of various electron-withdrawing monomers is realized by accurately regulating and controlling reaction conditions and alkyl magnesium substituent structures, and a series of magnesium polymers with controllable molecular weight distribution are successfully synthesized. The polymerization process shows typical living polymerization characteristics, the block copolymer with a regular structure is prepared through a sequential feeding strategy, modification of multiple functional end groups can be achieved, and a new technical approach is provided for designing and synthesizing high polymer materials with specific performance. A novel alkyl magnesium initiating system which is low in cost and easy to operate is provided for active anionic polymerization, the limitation of a traditional initiating system is broken through, the magnesium polymer with magnesium ions at the tail end is synthesized, a new technical path is provided for controllable preparation of high polymer materials, and important theoretical significance and wide industrial application prospects are achieved.

The invention provides a water-based polymer nano material as well as a preparation method and application thereof, and belongs to the technical field of nano materials. The preparation method of the water-based polymer nano material comprises the following steps: a hydrophilic monomer M1 is subjected to an active polymerization reaction in the presence of a compound A ', a water-soluble polymer P1-A is obtained, P1 is a water-soluble polymer main chain formed by a hydrophilic monomer M1 unit, and A is an active terminal formed by the compound A'; the water-soluble polymer P1-A and a monomer M2 are subjected to a polymerization reaction to obtain an amphiphilic block polymer P1-b-P2-A, and P2 is a hydrophobic block formed by a monomer M2 unit; in a water phase, an amphiphilic block polymer P1-b-P2-A is taken as a micelle seed, a hydrophobic monomer M3 is added, seed emulsion polymerization induced self-assembly is carried out in the presence of an initiator, and the water-based polymer nano material is obtained.

The invention discloses a double-terminal fluorescence labeled polymer as well as a preparation method and application thereof. The structural formula of the double-terminal fluorescence labeled polymer is shown as a formula V. In the formula V, n is 30-300, and x is 1-10. The preparation method comprises the following steps: carrying out ATRP (Atom Transfer Radical Polymerization) active polymerization reaction on a monomer by taking 2-bromo-2-methyl propionate 2-hydroxyethyl ester with hydroxyl at the tail end as an initiator to obtain a compound of which the tail end is terminated by hydroxyl and bromo; a hydroxyl terminal in the compound reacts with a perylene fluorescent dye shown in a formula II, a bromine terminal is subjected to an azidation reaction and then is subjected to a click chemical reaction with an ATTO647N dye, and the double-terminal fluorescence labeled polymer shown in a formula V is obtained. The double-fluorescent-molecule end-capped polymer disclosed by the invention has an FRET effect; the double-fluorescent-molecule-terminated polymer can realize single-molecule fluorescence microscopic imaging, and has important significance on basic researches such as micro-nano structure evolution of characterization and analysis materials and the like.

The application discloses a kind of anticorrosive easy-to-clean coatings for concrete structure, its preparation method and application method, belong to road anticorrosive coating production field.Anticorrosive easy-to-clean coatings are made of specific proportion water, water-based self-crosslinking emulsion, film forming aid, fumed silica, dispersing agent, hydrophobic modifier, wherein, the hydrophobic modifier is made by active polymerization reaction by fluorine-containing monomer, initiator, thioester chain transfer agent and hydrophilic monomer.Compared with prior art, the anticorrosive easy-to-clean coatings for concrete structure of the application has good easy-to-clean capacity while maintaining good durability, adhesion, and has good popularization and application value.

[Problem] Provided is a composition (slurry) which contains inorganic particles and water and in which sedimentation of the inorganic particles is suppressed. [Solution] This composition comprises inorganic particles, a copolymer (P) obtained by living polymerization, and water, and is characterized in that the copolymer (P) contains a structural unit (a-1) having a structure represented by formula (1) in a side chain and a structural unit (b-1) having an azole structure in a side chain.　(1): *-R13-(OR12)m1-OR11 [In formula (1), R11 represents a hydrogen atom or an alkyl group having 1-3 carbon atoms. R12 represents an alkylene group having 1-3 carbon atoms. R13 represents an alkylene group having 1-3 carbon atoms. m1 represents an integer of 0-30. When m1 is 2 or more, a plurality of the R12s may be the same as or different from each other. * represents a bond. ]

The invention relates to the technical field of high polymer material synthesis, and discloses a living polymerization method of liquid polyisoprene, which comprises the following steps: constructing a dynamic coordination network in normal hexane by using 0.05-0.15 part of a dilithium initiator and 5-8 parts of an ionic liquid containing bis (trifluoromethanesulfonimide) anions, adding 95-103 parts of an isoprene monomer, and carrying out a polymerization reaction to obtain the liquid polyisoprene. The preparation method comprises the following steps: carrying out living polymerization by adopting a gradient temperature program, introducing 0.5-1.5 parts of an end-capping reagent 5-15 minutes before the end of the reaction to realize double-end in-situ end capping, carrying out ethanol termination, centrifugal separation, normal hexane washing and drying to prepare double-end acrylate end-capped liquid polyisoprene, and recovering the ionic liquid for recycling. According to the method, side reaction is inhibited through a dynamic coordination network, a chain structure is regulated through the multi-stage action of the ionic liquid, stability is optimized through an end-capping collaborative model, the limitation of uncontrollability, extensive regulation and dynamic mismatch of a traditional process is broken through, and controllable synthesis of a high-purity polymer and a high-performance rubber material is achieved.

The application discloses a self-toughening block copolymer underfill adhesive, a preparation method and application, and belongs to the technical field of microelectronic packaging materials. The method comprises the following steps: preparing a rigid chain segment A prepolymer; obtaining a flexible chain segment B; performing an active polymerization reaction on the rigid chain segment A prepolymer and the flexible chain segment B to obtain a block copolymer; performing purification treatment on the block copolymer to remove unreacted substances and a catalyst, thereby obtaining a self-toughening block copolymer resin; and obtaining the self-toughening block copolymer underfill adhesive from the self-toughening block copolymer resin. The application further discloses the self-toughening block copolymer underfill adhesive prepared by the above method and application thereof. The self-toughening block copolymer underfill adhesive prepared by the application can fundamentally eliminate the problems of poor compatibility, easy precipitation and viscosity increase of an external toughening agent, and has low viscosity, high T g , high toughness and excellent long-term reliability, and can be widely applied to the field of advanced semiconductor packaging.

The invention belongs to the field of polymers, and particularly relates to a preparation method of a temperature-sensitive reversible dynamic covalent cross-linked polymer, which is obtained by polymerizing a monomer 1 containing more than two living polymerization units in a formula 1 and a monomer 2 containing more than two living polymerization units in a formula 2 (*-N = C = O), the temperature-sensitive reversible dynamic covalent cross-linked polymer containing the temperature-sensitive active fragment shown in the formula 3 is prepared. The invention also discloses the polymer prepared by the preparation method and application thereof. Innovative research shows that a cross-linked polymer with a structure shown as a formula 3 can be obtained by adopting a ring lactam structure shown as a formula 1 and a structure shown as a formula 2 for cross-linking polymerization, and the structure shown as the formula 3 can endow the prepared polymer with an excellent temperature-sensitive reversible transformation behavior; and the mechanical property, the self-repairing property, the multiple circulating recovery property and other performance characteristics can be improved.

This invention discloses a method for preparing cuprous oxide and multibranched polymer composite microcapsules. First, a prepolymer containing hydrophilic copper-complexing dimethylamino groups with epoxy end groups is synthesized using free radical living polymerization. Then, this prepolymer is condensed with polyamine molecules to prepare a multibranched block polymer, which is used as an additive in marine antifouling coatings. This additive polymer is blended with cuprous oxide nanoparticles, and based on the charge transfer effect between tertiary amines and copper, a composite microcapsule structure is formed, achieving encapsulation of copper antifouling agents. The advantages include effective control of copper antifouling agent release, while its multibranched structure increases the interaction force of the coating matrix resin, prolongs its residence time at the coating interface, and enhances the antifouling effect of the coating.

The application provides a B / P organic Lewis acid-base pair for catalyzing active polymerization of renewable vinyl monomers and a catalytic polymerization method thereof, and belongs to the technical field of polymer synthesis.The application realizes the active polymerization of renewable vinyl monomers by the synergistic catalysis of an organic boron Lewis acid and an organic phosphine Lewis base, realizes the active and controllable homopolymerization and copolymerization of different renewable vinyl monomers by adjusting the electronic effect and steric hindrance effect of the organic boron Lewis acid and the organic phosphine Lewis base, the molecular weight of the obtained polymer increases with the increase of the monomer to catalyst ratio, and the monomer conversion rate is 100%.Meanwhile, the B / P organic Lewis acid-base pair catalyst provided by the application is simple to synthesize and easy to commercialize, and the structure is rich in adjustability.The B / P organic Lewis acid-base pair catalyst provided by the application has a small amount in the catalytic reaction and is widely applicable to renewable monomers.

This invention discloses a RAFT reagent for catalyst-free photocontrolled polymerization of methyl methacrylate, its preparation method, and its application, belonging to the field of photocontrolled polymerization technology. The structure of the RAFT reagent is: ; R is selected from any of the following: The RAFT reagent of this invention, under visible light (green light, 520 nm) initiation, can achieve efficient and high-precision living polymerization of methyl methacrylate (MMA) without additional initiators or catalysts: the polymerization rate is twice that of the traditional RAFT reagent (CPDB), the induction period is shorter, the resulting polymer has an extremely narrow molecular weight distribution, and metal catalyst residue is completely avoided. This provides a key guarantee for the preparation of high-purity, structurally uniform polymers (such as high-performance photoresist resins), breaking through the technical bottlenecks of traditional high-temperature thermal polymerization or metal-catalyzed photocontrolled systems.

The invention discloses a preparation method of a gradient copolymer. [S = C (S-Z) S-R] trithiocarbonate is selected as a chain transfer agent, and the gradient copolymer is synthesized through an active polymerization reaction.

This invention discloses a selenium-thiolated RAFT reagent, its synthesis method, and its applications. The RAFT reagent is prepared by organic synthesis in the presence of selenium powder, sodium borohydride, carbon disulfide, and methyl 2-bromopropionate under an inert atmosphere. The RAFT reagent of this invention, as a chain transfer agent, is applied to the free radical polymerization of highly reactive acrylate monomers and less reactive styrene monomers, exhibiting living polymerization characteristics and good polymerization controllability. Selenides are used as regulators to synthesize organoselenium polymers with predetermined molecular weights, selenium content, and functional groups. The RAFT reagent has a light color, and the final polymer product is essentially free of RAFT reagent color.

The application discloses a preparation method of bottle brush polymer, comprising the following steps: heating norbornene-terminated polyester macromonomer to a molten state, adding a ROMP catalyst under the condition of containing a ligand to initiate a ring-opening metathesis polymerization reaction, and obtaining the bottle brush polymer; wherein the ligand is used for adjusting the activity of the ROMP catalyst, the polymerization reaction is carried out in a bulk system, and the content of the organic solvent in the bulk system is less than 8 wt%; and the ligand is pyridine. By adding the ligand (such as pyridine) into the reaction system, the initial activity of the Grubbs catalyst (such as G3) is effectively controlled, the catalyst is uniformly dispersed in the melt, then the norbornene-terminated polyester macromonomer is smoothly and controllably subjected to bulk ring-opening metathesis polymerization (ROMP) in a molten state, and the large amount of organic solvent required in traditional solution polymerization and the subsequent cumbersome removal process are avoided.

The invention discloses narrow-distribution liquid rubber based on a high-steric-hindrance silane chain transfer agent and a preparation method of the narrow-distribution liquid rubber, and relates to the technical field of liquid rubber. Through the combination of specifically designed high-steric-hindrance adamantyldimethylsilane and the specific solvent, the technical problem that high-efficiency chain transfer and high-fidelity re-initiation are difficult to simultaneously realize in a low-cost chain transfer agent system is creatively solved, so that the production cost is remarkably reduced; and a high-performance liquid rubber product comparable with the traditional expensive n-butyllithium'pure 'living polymerization is obtained.

The present disclosure provides a preparation method of a homogeneous rare earth catalyst. In the present disclosure, a depolymerizing agent is introduced into the homogeneous rare earth catalyst to promote complete depolymerization of an alkyl aluminum trimer into monomolecular alkyl aluminum. As a result, there is an increase in the number of the alkyl aluminum which serves as an effective chain transfer agent, resulting in a greatly improved chain transfer rate, such that a polymerization system has completed the chain transfer in an early stage of the reaction. Accordingly, an aluminum terminal molecular chain has an increased concentration, leading to an accelerated exchange with an active center propagating chain and a decreased influence caused by an increased viscosity of the system, maintaining living polymerization of the system.

The present application relates to a polymer synthesis method, in particular to a living polymerization method based on pulsed chain transfer. The polymerization method comprises chain transfer reaction stage and chain growth reaction stage alternately, and one chain growth reaction stage and one chain transfer reaction stage constitute a reaction cycle; in the chain transfer reaction stage, the whole reaction system is dominated by chain transfer reaction; in the chain growth reaction stage, the whole reaction system is dominated by the chain growth reaction of living polymerization; the living polymerization method further comprises a trigger condition, which makes the whole reaction system switch between the chain growth reaction stage and the chain transfer reaction stage; the trigger condition is a reaction condition which can be accurately controlled or a chemical condition which can be removed or changed. The present application can reduce the amount of living polymerization initiator and improve the controllability of the reaction system, and is especially suitable for preparing polymers with expected molecular weight distribution range or block polymers with expected sequence structure.