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Cationic polymerization method of alpha-methylstyrene/styrene copolymer

A technology of styrene copolymer and methyl styrene, which is applied in the field of polymer preparation technology, can solve the problems of low initiator activity, low molecular weight and high reaction efficiency, and achieves improved repeatability and stability and high monomer utilization rate. , The effect of simplifying the process

Active Publication Date: 2014-07-02
RACHEM CHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the prior art, the main problems in the synthesis method of the α-methylstyrene-styrene copolymer resin used as tire functional additives include: the synthetic α-methylstyrene / styrene copolymer, molecular weight and distribution , softening point, glass transition temperature and other indicators are difficult to meet at the same time; the composition and sequence distribution of α-methylstyrene / styrene copolymer is difficult to control; the activity and molecular weight of the initiator and the reaction efficiency are difficult to balance, for example, the initiator High activity means high reaction efficiency and high molecular weight; on the contrary, low initiator activity means low reaction efficiency and low molecular weight; raw material monomers need to be refined before use, and the repeatability and stability of the polymerization reaction are not good

Method used

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  • Cationic polymerization method of alpha-methylstyrene/styrene copolymer
  • Cationic polymerization method of alpha-methylstyrene/styrene copolymer
  • Cationic polymerization method of alpha-methylstyrene/styrene copolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] Weigh 177.27g of α-methylstyrene (molecular weight 118.18) and 156.21g of styrene (molecular weight 104.14), (α-methylstyrene: styrene molar ratio is 5: 5, and the total moles of monomers are 3), first place 3 / 4 of the amount of α-methylstyrene and all the styrene in a 500ml three-necked flask;

[0065] Take by weighing 150 grams of toluene and place the dropping funnel, the initiator system is made up of boron trifluoride etherate, ethanol, anhydrous phosphoric acid and phenetole, BF 3 : ethanol: phosphoric acid: the molar ratio of phenetole is 100: 100: 17.5: 11.5, BF 3 The molar ratio to the monomer is 0.2%, that is, 0.774ml of boron trifluoride etherate, 0.27g of ethanol, 0.1014g of phosphoric acid, and 0.084g of phenetole are added. Add them dropwise to the toluene solution, shake the dropping funnel to mix the initiator and toluene evenly.

[0066] Turn on the stirrer, add the mixed liquid of initiator and toluene dropwise, the dropwise addition is fast first an...

Embodiment 2

[0070] Weigh 248.18g of α-methylstyrene and 93.73g of styrene, (α-methylstyrene: styrene molar ratio is 7:3, the total number of moles of monomers is 3), the α-methylstyrene 2 / 3 of the styrene-based amount and all styrene are placed in a 500ml three-necked flask; 150 grams of toluene are weighed and placed in a dropping funnel, and the initiator system is made up of aluminum trichloride, ethanol, anhydrous phosphoric acid and anisole, Aluminum trichloride: ethanol: phosphoric acid: the mol ratio of anisole is 100: 50: 15: 10, and the mol ratio of aluminum trichloride and monomer is 0.2%, promptly adds 0.8g aluminum trichloride, 0.138g ethanol , 0.0882g phosphoric acid, 0.0649g anisole. Add them dropwise to the toluene solution, shake the dropping funnel to mix the initiator and toluene evenly. Other components and processing conditions are the same as in Example 1, and the experimental results are shown in Table 2.

Embodiment 3

[0072] Weigh 212.724g of α-methylstyrene and 124.968g of styrene, (α-methylstyrene: styrene molar ratio is 6:4, the total number of moles of monomers is 3), the α-methylstyrene 1 / 2 of the amount of base styrene and all the styrene are placed in a 500ml three-necked flask; 150 grams of toluene is weighed and placed in a dropping funnel, and the initiator system is composed of tin tetrachloride, ethanol, anhydrous phosphoric acid and phenetole, four Tin chloride: ethanol: phosphoric acid: the mol ratio of phenetole is 100: 30: 15: 10, and the mol ratio of tin tetrachloride and monomer is 0.15%, promptly adds 1.172g tin tetrachloride, 0.0621g ethanol, 0.0662 g phosphoric acid, 0.055 g phenetole. Add them dropwise to the toluene solution, shake the dropping funnel to mix the initiator and toluene evenly. The reaction temperature was controlled at about 40°C, and the time for dropping the initiator was controlled at about 30 minutes. Other components and process conditions were th...

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Abstract

The invention discloses a cationic polymerization method of an alpha-methylstyrene / styrene copolymer represented by formula (I). The method comprises the following steps: 1, adding an alpha-methylstyrene monomer and a styrene monomer into a polymerization container, and uniformly mixing, wherein a molar ratio of the alpha-methylstyrene monomer to the styrene monomer is 0.3-5; 2, adding an initiator into an organic solvent in order to prepare an initiator solution, wherein the initiator is anyone of Lewis acids, alcohols, protonic acids or ethers; and 3, adding the initiator solution into a mixed solution obtained in step 1, and carrying out a polymerization reaction in order to obtain the alpha-methylstyrene / styrene copolymer. The method has the advantages of omission of monomer refining and water washing steps, and a high reaction yield, and the alpha-methylstyrene / styrene copolymer prepared in the invention can be added to tread rubber in order to improve the grip and the wear resistance of treads, and has the effects of a tackifier and a softening agent.

Description

technical field [0001] The invention relates to the field of polymer preparation technology, in particular to a cationic polymerization method of alpha-methylstyrene / styrene copolymer. Background technique [0002] α-Methylstyrene and styrene copolymer resins are widely used as tackifiers, softeners, wetting agents, and fillers in coatings, adhesives, synthetic rubber, sealants, and caulking agents, and have good thermal stability , compatibility and solubility, and also has the advantages of single component, no solvent, low odor, light color, etc., so it has a very broad application prospect in various fields of the chemical industry and has a large market development space. [0003] There are few reports on the copolymerization of styrene and α-methylstyrene at home and abroad. The current published literature shows that the research on a-methylstyrene / styrene copolymerization mainly lies in free radical copolymerization and anionic copolymerization, but the molecular we...

Claims

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Application Information

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IPC IPC(8): C08F212/06C08F212/08C08F4/14C08F2/06
Inventor 李卞
Owner RACHEM CHINA CO LTD