Preparation method of cationic type fluorine-containing soap-free emulsion

A soap-free emulsion and cationic technology, which is used in the field of soap-free emulsion and leather finishing preparation, can solve the problems of reduced polymer product performance, uncontrollable molecular weight, wide molecular weight distribution, etc., and achieves improved performance, good stability, Small particle size distribution effect

Active Publication Date: 2015-11-04
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, in traditional RAFT emulsion polymerization, the emulsion prepared by using small molecule RAFT reagents has the problems of poor polymerization stability, uncontrollable molecular weight and wide molecular weight distribution, and the presence of a large amount of emulsifier in the final emulsion product will reduce the performance of the polymer product

Method used

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  • Preparation method of cationic type fluorine-containing soap-free emulsion
  • Preparation method of cationic type fluorine-containing soap-free emulsion
  • Preparation method of cationic type fluorine-containing soap-free emulsion

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preparation example Construction

[0050] The preparation method of a cationic fluorine-containing soap-free emulsion of the present invention is specifically implemented according to the following steps:

[0051] Step 1. Weigh azobisisobutyronitrile, N,N dimethylaminoethyl methacrylate, 1,4-dioxane, S-1 respectively according to the mass ratio of 1:39 to 90:143:3 - dodecyl-S'-(α,α"-dimethyl-α"-acetic acid) trithiocarbonate;

[0052] Step 2, using the azobisisobutyronitrile, N,N dimethylaminoethyl methacrylate, 1,4-dioxane, S-1-dodecyl-S'- (α, α "-dimethyl-α "-acetic acid) trithiocarbonate is prepared to obtain polymethacrylate N, N dimethylaminoethyl ester (also known as: PDMAEMA-RAFT), specifically according to the following steps:

[0053] Step 2.1, at room temperature, the azobisisobutyronitrile, N,N dimethylaminoethyl methacrylate, 1,4-dioxane, S-1-dodecane weighed in step 1 Base-S'-(α, α"-dimethyl-α"-acetic acid) trithiocarbonate is added together in a three-necked flask equipped with a magnet;

[0054...

Embodiment 1

[0083] Weigh azobisisobutyronitrile, N,N dimethylaminoethyl methacrylate, 1,4-dioxane, S-1-dodecyl respectively according to the mass ratio of 1:39:143:3 -S'-(α,α"-dimethyl-α"-acetic acid) trithiocarbonate;

[0084] At room temperature, the weighed azobisisobutyronitrile, N,N dimethylaminoethyl methacrylate, 1,4-dioxane, S-1-dodecyl-S'-( α, α″-dimethyl-α″-acetic acid) trithiocarbonate was added together in a three-necked flask equipped with a magnet; wherein, the three necks of the three-necked flask were connected from left to right with a thermometer, reflux condensing Pipe, air guide tube; first pass argon gas into the three-necked flask for 20 minutes, and then heat the three-necked flask to 70°C under the state of argon gas, so that the azobisisobutyronitrile and methacrylic acid in the three-necked flask N, N Dimethylaminoethyl ester, 1,4-dioxane, S-1-dodecyl-S′-(α,α″-dimethyl-α″-acetic acid) trithiocarbonate in argon Protect and react, the reaction time is 6h, to obta...

Embodiment 2

[0089] Weigh azobisisobutyronitrile, N,N dimethylaminoethyl methacrylate, 1,4-dioxane, S-1-dodecyl respectively according to the mass ratio of 1:50:143:3 -S'-(α,α"-dimethyl-α"-acetic acid) trithiocarbonate;

[0090] At room temperature, the weighed azobisisobutyronitrile, N,N dimethylaminoethyl methacrylate, 1,4-dioxane, S-1-dodecyl-S'-( α, α″-dimethyl-α″-acetic acid) trithiocarbonate was added together in a three-necked flask equipped with a magnet; wherein, the three necks of the three-necked flask were connected from left to right with a thermometer, reflux condensing Tube, air guide tube; first pass argon gas into the three-necked flask for 25 minutes, and at this time 1,4-dioxane is used as a solvent; then, under the state of re-passing argon gas, heat the three-necked flask to 75°C to make the three-necked flask Azobisisobutyronitrile, N,N dimethylaminoethyl methacrylate, 1,4-dioxane, S-1-dodecyl-S'-(α,α"-dimethyl- α″-acetic acid) trithiocarbonate was reacted under the...

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Abstract

The invention discloses a preparation method of a cationic type fluorine-containing soap-free emulsion. The preparation method comprises the steps: using azodiisobutyronitrile, 2-(dimethylamino)ethyl methacrylate, 1,4-dioxane, S-1-dodecyl-S'-(alpha,alpha''-dimethyl-alpha''-acetic acid)trithiocarbonate to prepare poly[2-(dimethylamino)ethyl methacrylate]; purifying poly[2-(dimethylamino)ethyl methacrylate] for two times with n-hexane, and drying to obtain a product after purification; dissolving the product after purification in diluted hydrochloric acid, and forming a mixed solution; preparing an amphiphilic block copolymer from the mixed solution, 2,2'-azobis[2-methylpropionamidine]dihydrochloride, a hexafluorobutyl acrylate agent and deionized water; and combining the prepared mixed monomer with the amphiphilic block copolymer and an initiator aqueous solution to prepare the cationic type fluorine-containing soap-free emulsion. The fluorine-containing soap-free emulsion obtained by the preparation method disclosed by the invention has the characteristics of good stability, small latex particle size, and core-shell structure.

Description

technical field [0001] The invention belongs to the technical field of preparation methods of leather finishing agents, and relates to a soap-free emulsion for finishing leather, in particular to a preparation method of a cationic fluorine-containing soap-free emulsion. Background technique [0002] In recent years, "living" / controllable radical polymerization methods are being gradually developed, such as: atom transfer radical polymerization (ATRP), nitroxide stabilized radical polymerization (NMRP), reversible addition-fragmentation transfer radical ( RAFT) polymerization, etc.; among them, the experimental conditions of RAFT polymerization are basically the same as those of traditional free radical polymerization, and the applicable range of monomers is wide. Realized polymerization, considered one of the most industrially potential "living" / controlled radical polymerization techniques, has been widely used in emulsion polymerization and miniemulsion polymerization. [...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/14C08F220/18C08F220/22C08F2/28C08F293/00C08F220/34C08F2/38
Inventor 周建华李艳南王海龙马建中贺仁妍
Owner SHAANXI UNIV OF SCI & TECH
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