Method for regulating and controlling silk graft copolymerization reaction on basis of hydrophobic and hydrophilic performance of free radicals

A hydrophilic and hydrophobic, copolymerization technology, applied in the field of silk grafting, can solve the problems of unfavorable industrial production, complex process, large gap, etc., and achieve the effects of convenient implementation, simple operation and easy acquisition.

Inactive Publication Date: 2013-06-12
ZHEJIANG SCI-TECH UNIV
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  • Abstract
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  • Claims
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Problems solved by technology

The Chinese patent No. ZL 200810019560.6 discloses a method for preparing functional real silk. Firstly, a real silk macromolecular initiator is prepared, and then a graft copolymerization reaction is carried out. However, the process of preparing the real silk macromolecular initiator is complicated, and The preparation of silk macromolecular initiators and graft copolymerization need to be carried out in organic solvents, which is far behind the existing industrial technology
In addition, by radiation method (Jing Zhang. The surface characterization of mulberry silk grafted with acrylamide by plasma copolymerization, J.Appl.Polym.Sci., 1997, 48:1713-1717; A.S.Bashiar, Mubarak A.Khan and K.M.Idriss Ali .Modification of cotton, rayon and silk fibers by radiation induced graft co-polymerization, Radia.Phys.Chem., 1995, 45 (5): 753-759.) and photoinitiation (Subasini Lenka, Padma L.Nayak, and Munmay K.Mishira.Photo-induced graft copolymerization, I.Graft copolymerization of methyl methacrylate onto silk in presence of lutidine-bromine charge transfer complex, Die Angewandte Makromolekulare Chemie, 1981, 99:45-54; Bashar, Mubarak A.Khan, K.M. Idriss Ali.Modification of cotton, rayon, and silk with urethane acrylate under ultraviolet radiation, J.Appl.Polym.Sci., 1997, 63:1703-1711.) etc., can also regulate the generation reaction of free radicals, and even Free radicals are limited to the surface of silk fibroin, but compared with chemical initiation, the above two initiation methods have significantly higher requirements on reaction conditions and equipment, which is not conducive to industrial production

Method used

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  • Method for regulating and controlling silk graft copolymerization reaction on basis of hydrophobic and hydrophilic performance of free radicals
  • Method for regulating and controlling silk graft copolymerization reaction on basis of hydrophobic and hydrophilic performance of free radicals
  • Method for regulating and controlling silk graft copolymerization reaction on basis of hydrophobic and hydrophilic performance of free radicals

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0093] (1) Preparation of 2-(dodecyl trithiocarbonate group) propionic acid

[0094]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, 38...

Embodiment 2

[0101] (1) The preparation of 2-(dodecyl trithiocarbonate group) propionic acid is the same as in Example 1.

[0102] (2) preparation of the trithiocarbonate compound of formula V structural formula

[0103] Put the following reagents into a 500mL three-necked flask equipped with a reflux condenser, a nitrogen inlet, and a feed port: 28 grams of dioxane, 1.25 grams of yellow flaky crystals prepared in step (1), and 0.098 grams of azodicyanovaleric acid. grams and 3.34 grams of styrene. After passing high-purity (99.99%) nitrogen to the above device for 1 hour, immerse in a water bath at 80° C., and after 12 hours, an intermediate product was obtained; continue to add 18 grams of dioxane and 0.067 grams of azodicyanovaleric acid to the three-necked flask 1. 6.94 grams of acrylic acid, continued to react in a water bath at 80° C. for 8 hours, then lowered the temperature, stopped the reaction, and obtained a reaction product. The reaction product was poured into 200 mL of cycl...

Embodiment 3～20

[0108] Refer to Table 1 for the raw materials involved in Examples 3-20, the amount of raw materials used, and the reaction conditions of the copolymerization reaction. Weigh the dried refined silk and the trithiocarbonate compound, and put the two into a 50mL reaction bottle Add water, water-soluble monomers required for graft copolymerization and formic acid aqueous solution to the bottle, then place the reaction bottle in a oscillating water bath, and turn on the power of the water bath; when the temperature rises to the preset value of the copolymerization reaction When the temperature is 70°C-90°C, put an initiator into the reaction bottle to initiate the copolymerization reaction. After reacting at 70°C-90°C for 0.5h-2.0h, take out the primary silk grafted with water-soluble polymer and wash it with 100mL pure water Put into the 150mL washing bottle after washing, add soaping solution in bottle (soaping solution is the soda ash and 0.03% sodium hydrosulfite containing 0.0...

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Abstract

The invention discloses a method for regulating and controlling a silk graft copolymerization reaction on the basis of hydrophobic and hydrophilic performance of free radicals. A trithiocarbonic ester compound is used for regulating and controlling a water-phase silk graft copolymerization reaction, and the trithiocarbonic ester compound is a compound having the structure represented by the formula I or formula II, wherein y is from 1 to 5, x is from 10 to 50, n is from 4 to 12, and x, y and n are integral numbers. The water-phase silk graft copolymerization reaction is regulated and controlled by adding the trithiocarbonic ester compound, so that the grafting efficiency of monemers can be increased, and the purpose of improving the weight gain of silk grafts is achieved. With the method for regulating and controlling the silk graft copolymerization reaction on the basis of hydrophobic and hydrophilic performance of free radicals, only simple improvements are made on the basis of the industrially mature silk graft copolymerization reaction, so that the method is easy to operate and convenient to implement. The formula I and the formula II are disclosed in the specification.

Description

technical field [0001] The invention relates to the field of silk grafting, in particular to a method for regulating silk graft copolymerization based on free radical hydrophilicity and hydrophobicity. Background technique [0002] In industry, the graft copolymerization reaction of silk is usually carried out with water as the medium, and the reaction system has obvious heterogeneous characteristics. During this process, since the initiator and the monomer are water-soluble, both the monomer and the initiator required in the graft copolymerization reaction need to migrate from the water phase to the silk to maintain the reaction. Accompanied by the graft copolymerization reaction is the homopolymerization reaction in aqueous phase. Since the homopolymerization reaction consumes monomers and the generated homopolymer does not contribute to the graft copolymerization, it should be avoided as a side reaction. [0003] S. Lenka et al. (Grafting Vinyl Monomers onto Silk Fibers,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D06M14/06
Inventor 杨雷刘文文周利展沈一峰戚栋明
Owner ZHEJIANG SCI-TECH UNIV
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