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Double-terminal olefinic bond terminated polyether and synthesis method thereof

A technology of capping polyether and its synthesis method, which is applied in the field of polymer preparation, can solve the problems of high initiator and capping agent, consumption price, complex process, etc., and achieve good mechanical properties, cost saving, and simple process Effect

Pending Publication Date: 2021-03-12
南京清研新材料研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The overall process is complicated, and it needs to consume relatively expensive initiators and end-capping agents

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 0.52 g of ethylene glycol, 18.4 g of pulverized KOH with a purity of 95%, and 349 g of propylene oxide in a pressure-resistant stainless steel reactor with heating, cooling and stirring. Oxygen in the system was replaced with nitrogen. Stir at high speed to fully disperse KOH. Heating to 60°C, the reaction starts, the system releases heat, stop heating, remove the reaction heat in time by cooling, control the system temperature at 60°C, and the fluctuation does not exceed 5°C. After reacting for 8 hours, the system pressure dropped to 0 MPa. 10.4 g of dichloromethane was sucked in by vacuum, and reacted at 55° C. for 3 hours, and then 23.4 g of chloropropene was sucked in by vacuum, and reacted at 70° C. for 3 hours. After the reaction product was centrifuged to separate the solid, 11 mL of 17% phosphoric acid was added, and the pH value was measured to be 6.5. The water was evaporated under reduced pressure at 130° C., and then centrifuged again. A transparent v...

Embodiment 2

[0027] Add 0.52g of ethylene glycol, 18.4g of pulverized KOH with a purity of 95%, and 348g of propylene oxide in a pressure-resistant stainless steel reactor with heating, cooling and stirring. Oxygen in the system was replaced with nitrogen. Stir at high speed to fully disperse KOH. Heating to 40°C, the reaction starts, the system releases heat, stop heating, remove the reaction heat in time by cooling, control the system temperature at 40°C, and the fluctuation does not exceed 1°C. After 24 hours of reaction, the system pressure dropped to 0 MPa. 21 g of dichloromethane was sucked in by vacuum, and reacted at 55° C. for 3 hours, and then 23.4 g of chloropropene was sucked in by vacuum, and reacted at 70° C. for 3 hours. After the reaction product was centrifuged to separate the solid, 7 mL of 17% phosphoric acid was added, and the pH value was measured to be 6. The water was evaporated under reduced pressure at 130° C., and centrifuged again. A transparent viscous polyme...

Embodiment 3

[0029] Add 3.63 g of ethylene glycol, 36.8 g of pulverized KOH with a purity of 95%, and 348 g of propylene oxide in a pressure-resistant stainless steel reactor with heating, cooling and stirring. Oxygen in the system was replaced with nitrogen. Stir at high speed to fully disperse KOH. Heating to 40°C, the reaction starts, the system releases heat, stop heating, remove the reaction heat in time by cooling, control the system temperature at 40°C, and the fluctuation does not exceed 1°C. After 16 hours of reaction, the system pressure dropped to 0 MPa. 21 g of dichloromethane was sucked in by vacuum, and reacted at 55° C. for 7 hours, and then 5.1 g of chloropropene was sucked in by vacuum, and reacted at 60° C. for 5 hours. After the reaction product was centrifuged to separate the solid, 5 mL of 17% phosphoric acid was added, and the pH value was measured to be 6. The water was evaporated under reduced pressure at 130° C., and then centrifuged again. A transparent viscous...

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Abstract

The invention relates to double-terminal olefinic bond terminated polyether with a structural general formula of CH2 = CH-CH2-O- (CH (CH3)-CH2-O) m-(CH2O) n-CH2CH = CH2 and a synthetic method thereof.The synthetic method comprises the following steps that 1, oxygen is removed through nitrogen replacement, dihydric alcohol is added to serve as an initiator, epoxypropane is added under KOH catalysis, and high-speed stirring is performed to fully disperse KOH in a system; heating is performed to carry out ring-opening polymerization reaction on epoxypropane; 2, dichloromethane is added, and molecular chain extension is completed; 3, chloropropene is added, and allyl end capping is completed; 4, unreacted KOH and solid by-products in the system are removed; and 5, the pH value is regulated, and water, the solvent and the solid in the system are removed to obtain the transparent viscous double-terminal olefinic bond terminated polyether. According to the invention, allyl spontaneously generated by a chain transfer reaction in an epoxypropane polymerization process is used as a double bond source, an allyl alcohol initiator is not used, and only a small amount of chloropropene is used as a final end capping agent. The process is simple, the cost is saved, and large-scale production is easy to realize.

Description

technical field [0001] The invention relates to the field of polymer preparation, in particular to a double-terminal ethylenic bond-terminated polyether and a synthesis method thereof. Background technique [0002] Double-terminal ethylenic bond-terminated polyether, the general method is to polymerize allyl alcohol as an initiator to obtain a single-terminated polyether, and then use allyl chloride to end-cap under the catalysis of a strong base. The present invention breaks through this idea, does not use allyl alcohol initiator, and uses allyl group produced by chain transfer reaction in the polymerization process of propylene oxide as the main source of double bonds. [0003] The prior art uses allyl alcohol starter, which needs to prepare potassium allyl alcohol. After preparing the single-capped polyether, it is necessary to use KOH to treat the polyether and allyl chloride to undergo a Williamson reaction for capping. On the whole, the process is complicated, and ex...

Claims

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Application Information

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IPC IPC(8): C08G65/337C08G65/28
CPCC08G65/337C08G65/2609C08G2190/00
Inventor 张奇张新
Owner 南京清研新材料研究院有限公司
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