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Trithiocarbonate compound containing ethylene, preparation method and application thereof

A technology of trithiocarbonates and compounds, which is applied in the field of preparation of trithiocarbonates, can solve the problems of difficulty in obtaining continuous structure membrane materials, difficulty, and restrictions on the promotion and application of new membrane materials, and achieve good application prospects, Easy to adjust, suitable for a wide range of monomer effects

Inactive Publication Date: 2013-03-20
ZHEJIANG SCI-TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, due to the participation of the divinyl monomer in the polymerization reaction, the polymer chains in the microspheres are cross-linked, so that the resulting polymers are neither soluble nor meltable, so that the polymer chains between the microspheres diffuse each other during film formation. It is very difficult to obtain membrane materials with continuous structure
These shortcomings restrict the promotion and application of new membrane materials to a large extent.

Method used

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  • Trithiocarbonate compound containing ethylene, preparation method and application thereof
  • Trithiocarbonate compound containing ethylene, preparation method and application thereof
  • Trithiocarbonate compound containing ethylene, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] (1) Preparation of 2-(dodecyl trithiocarbonate group) propionic acid

[0058] Mix 10 grams of sodium hydroxide, 5.4 grams of tetrapropylammonium bromide and 10 grams of water uniformly at room temperature, add them to a 500 mL three-necked round-bottomed flask with a stirring bar and stir, and protect the reaction system with nitrogen gas. 60mL of dodecanethiol was added dropwise into a three-necked round-bottomed flask with a syringe, and the reaction was continued for 0.5 hours after the dropwise addition; During the dropwise addition, it can be observed that white flocs are generated and gradually increase. After the dropwise addition, the reaction is kept for 0.5 hours, and then ice bathed. After the temperature of the material in the reactor was completely lowered to 0°C, 15 mL of carbon disulfide was added dropwise into the flask with a syringe, and the reaction solution turned into a yellow turbid solution at this time. After keeping the reaction for 0.5 hour, 3...

Embodiment 2

[0063] (1) The preparation of 2-(dodecyl trithiocarbonate group) propionic acid is the same as in Example 1.

[0064] (2) Preparation of vinyl-containing trithiocarbonate compounds

[0065] In a 250mL three-necked flask equipped with a reflux condenser, a nitrogen inlet, and a feed port, drop the following reagents: 5 grams of dioxane, 2-(dodecyltrithiocarbonate) propane prepared in step (1) Acid 0.3 g, azodicyanovaleric acid 0.025 g and N, N'-dimethylacrylamide 4.0 g. After passing high-purity (purity: 99.99%) nitrogen to the above device for 1 hour, immerse in a 70°C water bath, and after 10 hours, an intermediate product was obtained; continue to add 1 gram of dioxane and azodicyanovaleric acid to the three-necked flask 0.025 g, 0.97 g of a dienyl double bond-containing monomer with the structure of formula 20 was continued to react in a water bath at 80° C. for 12 hours, then the temperature was lowered, and the reaction was stopped to obtain the product. The product was...

Embodiment 3

[0068] (1) Preparation of 2-(dodecyl trithiocarbonate group) isobutyric acid

[0069] Add 202.4 grams of mercaptan, 16.14 grams of methyl trioctyl ammonium chloride and 482.06 grams of acetone into a three-necked flask with a reflux condensing device, the temperature of the water bath is 10 ° C, magnetic stirring, nitrogen, and deoxygenation for 20 minutes Add dropwise the sodium hydroxide aqueous solution of 40 grams (mass concentration is 50%), add in 20 minutes, continue reaction 15 minutes; Add dropwise the acetone mixed solution of the carbon disulfide of 76.1 grams and 98.74 grams, after adding in 20 minutes, Continue to react for 10 minutes; Add 179.07 grams of chloroform, then dropwise add 200 grams of sodium hydroxide aqueous solution (mass concentration is 50%), dropwise in 0.5 hours, stir and react for 12 hours; Add 1500 grams of deionized water, Then add 109.5 grams of concentrated hydrochloric acid (mass concentration is about 37%); blow nitrogen, stir vigorously,...

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Abstract

The invention discloses a trithiocarbonate compound containing ethylene, which is the compound with a structure in the formula I or II, and the ethylene is positioned between the hydrophilic chain segment and the hydrophobic chain segment of the compound. The invention further discloses a preparation method of the trithiocarbonate compound containing the ethylene, under the action of a radical initiator, the compound with the structure in the formula III or VI is firstly reacted with a water-soluble monomer with a chain link A or a chain link C, and is secondarily reacted with a monomer containing a diene double linkage, so the compound with the structure in the formula I or II is obtained; and the preparation method has the characteristics of simple preparation, strong operability, good reproducibility and the like. The invention also discloses the application of the trithiocarbonate compound containing the ethylene in preparing polymer microspheres, so the ethylene is gathered at the surfaces of the polymer microspheres.

Description

technical field [0001] The invention relates to the field of preparation of trithiocarbonate compounds, in particular to a vinyl-containing trithiocarbonate compound and its preparation method and application. Background technique [0002] Studies have shown that the performance of polymer materials is not only determined by chemical composition, but also largely determined by the structure of polymer chains. The preparation of polymer materials with precise molecular chain structure, so as to control the properties of materials at the molecular level, is of great significance for improving the performance of polymer materials and increasing the functions of polymer materials. Among them, the chemical reaction of functional groups participating in specific positions in the polymer chain has become an important method for designing the composition of polymer materials and the structure of polymer chains (Takemoto K., Ottenbrite R.M., Kamachi M.Functional Monomers and Polymers...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F220/06C08F220/56C08F290/12C08F212/08C08F220/18C08F2/24B01J13/14
Inventor 杨雷杨海刘文文胡承杰
Owner ZHEJIANG SCI-TECH UNIV
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