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Chain transfer agent with flame retardance and preparation method thereof

A technology of chain transfer agent and flame retardancy, which is applied in the field of chain transfer agent with flame retardancy and its preparation, can solve the problems of easy loss of flame retardant, no flame retardancy, poor dispersibility, etc. Inexpensive, reduced scuffing and wear, and easy-to-use synthetic process

Inactive Publication Date: 2020-10-30
李太杰
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Most polymer materials are not flame retardant, such as polyethylene, polypropylene, polystyrene, etc. In order to make the obtained polymer material flame retardant, some flame retardants are usually added to make the polymer material flame retardant. Flammability, on the one hand, the added flame retardant may have poor compatibility with the polymer material, poor dispersion, and on the other hand may have the problem of easy loss of the flame retardant. Based on this, the present invention prepares a flame retardant RAFT chain transfer agent, when the RAFT chain transfer agent is used to initiate the copolymerization of the monomer, the copolymerized material has flame retardancy, and there is no need to add a flame retardant to the polymer material

Method used

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  • Chain transfer agent with flame retardance and preparation method thereof
  • Chain transfer agent with flame retardance and preparation method thereof
  • Chain transfer agent with flame retardance and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023]

[0024] Add 3-benzylmercaptothiocarbonylpropionic acid (5mmol) into a 100mL branched-necked flask, add 30mL of dichloromethane, slowly add thionyl chloride (7.5mmol) dropwise, react at 40°C for 1.5h, remove low pressure under reduced pressure The boiling point residue was extracted with ethyl acetate / water, the combined organic phases were washed with water, brine, Na 2 SO 4 Dry, filter and concentrate with 10% EtOAc-n-hexane (v / v) as the eluent, and column purification to obtain 3-benzylmercaptothiocarbonylpropionic acid chloride with a yield of 85.4%.

Embodiment 2

[0026]

[0027] Add 1,3,5-tris(2-hydroxyethyl)cyanuric acid (5mmol) into a 100mL branched-necked flask, add 20mL of dichloromethane, raise the temperature to 40°C, add pyridine (5mmol) and acid chloride 3-benzene A dichloromethane solution of methylmercaptothiocarbonyl propionic acid (5 mmol) was reacted at 40°C for 3 h. After the reaction was completed, it was extracted with ethyl acetate / water, and the combined organic phases were washed with water and brine, and Na 2 SO 4 After drying, filtering and concentrating, 5% EtOAc-n-hexane (v / v) was used as the eluent, and the column was purified to obtain the flame-retardant chain transfer agent 1a with a yield of 88.1%. 1 H-NMR (400MHz, CDCl 3 ),δ(ppm):7.31-7.25(m,5H,Ph),4.82(s,2H,OH),4.60(s,2H,CH 2 ),4.51(t,2H,CH 2 ),3.63(t,4H,CH 2 ),3.45(t,2H,CH 2 ),3.38(t,4H,CH 2 ),3.27(t,2H,CH 2 ),2.89(t,2H,CH 2 ). 13 C-NMR (100MHz, CDCl 3 ), δ(ppm): 226.31, 171.45, 148.32, 136.15, 128.78, 127.72, 127.21, 60.10, 57.24, 47.83, 45....

Embodiment 3

[0029]

[0030] Add 1,3,5-tris(2-hydroxyethyl)cyanuric acid (5mmol) into a 100mL branched-necked flask, add 20mL of dichloromethane, raise the temperature to 40°C, add pyridine (10mmol) and acid chloride 3-benzene A dichloromethane solution of methylmercaptothiocarbonyl propionic acid (10 mmol) was reacted at 40°C for 3 h. After the reaction was completed, it was extracted with ethyl acetate / water, and the combined organic phases were washed with water and brine, and Na 2 SO 4 After drying, filtering and concentrating, 5% EtOAc-n-hexane (v / v) was used as the eluent, and the column was purified to obtain flame-retardant chain transfer agent 2a with a yield of 82.4%. 1 H-NMR (400MHz, CDCl 3 ),δ(ppm):7.38-7.26(m,10H,Ph),4.91(s,1H,OH),4.67(s,4H,CH 2 ),4.55(t,4H,CH 2 ),3.75(t,2H,CH 2 ),3.53(t,4H,CH 2 ),3.46(t,2H,CH 2 ),3.32(t, 4H,CH 2 ),2.91(t,4H,CH 2 ). 13 C-NMR (100MHz, CDCl 3 ), δ(ppm): 227.24, 172.14, 149.85, 136.96, 129.52, 128.46, 127.87, 61.24, 57.97, 49.20, 45....

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Abstract

The invention discloses a chain transfer agent with flame retardance and a preparation method thereof. The chain transfer agent with the flame retardance is prepared by the steps: carrying out acylating chlorination reaction on 3-phenylmethylmercaptothiocarbonyl propionic acid, and carrying out condensation reaction on the 3-phenylmethylmercaptothiocarbonyl propionic acid and 1,3,5-tri(2-hydroxyethyl) cyanuric acid, so as to obtain the chain transfer agent with the flame retardance. The synthesis process for preparing the chain transfer agent with flame retardance is simple to operate, no toxic by-product is generated, the synthesis raw materials are low in price, the prepared chain transfer agent has a good flame retardant effect, and the obtained chain transfer agent has good wear resistance as a lubricating oil additive.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a flame-retardant chain transfer agent and a preparation method thereof. Background technique [0002] RAFT polymerization is based on the addition of the propagating free radical to the double bond of the compound containing -S-C=S structure, and the S-C bond is broken to introduce a reversible chain transfer reaction to realize the active growth of the polymer chain, so it is called reversible addition-break chain Transfer radical polymerization. The biggest advantage of RAFT is that it is applicable to a wide range of monomers. In addition to common monomers, acrylic acid, sodium p-vinylbenzenesulfonate, hydroxyethyl methacrylate, aminoethyl methacrylate and other protonic monomers or acids, Basic monomers can be polymerized smoothly, which is very beneficial to the polymerization reaction of ethylenic monomers containing special functional groups. There is no n...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D251/32C08F112/08C08F2/38
CPCC07D251/32C08F112/08C08F2/38
Inventor 李太杰
Owner 李太杰
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