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Synthesis method of unsaturated polyoxyethylene ether containing aerobic heterocyclic alkane and product and application of unsaturated polyoxyethylene ether

A technology of oxetane and polyoxyethylene ether, which is applied in the application field of preparing polycarboxylate water reducer, can solve the problem of increasing the complexity and uncertainty of free radical copolymerization reaction, unfavorable large-scale industrial production, difficult Quantitative control and other issues, to achieve excellent retarding effect, broad application prospects and market potential, high expansion effect

Active Publication Date: 2017-10-17
SHANGHAI TAIJIE CHEM
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  • Description
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Problems solved by technology

[0005] In the prior art, straight-chain unsaturated polyoxyethylene ether synthesized polycarboxylate water-reducer mainly acts as steric hindrance to improve the dispersibility of cement particles. However, the polycarboxylate water-reducer The electrostatic repulsion shown is small; in addition, in the prior art, the introduction of phenyl functional groups and heterocyclic functional groups can improve the retarding performance of polycarboxylate superplasticizers and prolong the initial and final setting times of concrete. , it is often necessary to add phenyl or heterocyclic reactants with copolymerization activity during the polymerization reaction to participate in the free radical copolymerization reaction, which increases the complexity and uncertainty of the free radical copolymerization process. The reaction is difficult to control quantitatively, so it is not conducive to large-scale industrial production

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  • Synthesis method of unsaturated polyoxyethylene ether containing aerobic heterocyclic alkane and product and application of unsaturated polyoxyethylene ether
  • Synthesis method of unsaturated polyoxyethylene ether containing aerobic heterocyclic alkane and product and application of unsaturated polyoxyethylene ether
  • Synthesis method of unsaturated polyoxyethylene ether containing aerobic heterocyclic alkane and product and application of unsaturated polyoxyethylene ether

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preparation example Construction

[0029] According to the first aspect, the synthesis method of unsaturated polyoxyethylene ether containing oxetane comprises the following steps: S1: taking the oxetane with terminal hydroxyl as the starting material, adding the oxetane with terminal hydroxyl Put cycloalkane in the reaction vessel, stir rapidly, slowly introduce chlorine gas, and react at 65°C-85°C for 45min-90min under the condition of ultraviolet light irradiation, complete the chlorination reaction, and obtain intermediate A; S2: prepare from S1 Add the Grignard reagent containing C2-C10 straight-chain alkenyl to the obtained intermediate A, and stir the reaction at 5°C-35°C for 30min-90min; post-treatment to obtain intermediate B; S3: prepare S2 The obtained intermediate B is placed in a pressurized reaction device, and an anionic ring-opening polymerization catalyst and ethylene oxide or / and propylene oxide are added, at 145 ° C to 185 ° C and at 2.0 times to 3.0 times the standard atmospheric pressure Un...

Embodiment 1

[0052] Put 1000g of tetrahydrofuran-3-methanol in a reaction container, stir rapidly, and slowly introduce chlorine gas, and react in a UV reaction box at 75°C for 45min to obtain intermediate A: 4-chloro-tetrahydrofuran-3-methanol .

[0053] Add 1000g of intermediate A to another reaction device, and then add 700g of Grignard reagent R'MgCl, wherein R' is vinyl; the reaction temperature is 25°C, and the reaction is stirred for 65min; the reaction is complete, post-treatment, and the intermediate is obtained B: 4-vinyl-tetrahydrofuran-3-methanol.

[0054] Add 500g of intermediate B into a pressurized reaction device with a volume of 10L, and add 50g of sodium methoxide as a catalyst, add 6000g of ethylene oxide (EO), stir the reaction and control the reaction temperature to 165°C and the reaction pressure to 2.0 times the standard Atmospheric pressure, the reaction time is 5.5h. After the reaction, the temperature was lowered to 55° C., and then an appropriate amount of glac...

Embodiment 2

[0056] Put 1100g of tetrahydrofuran-2-ethanol in the reaction container, stir rapidly, and slowly introduce chlorine gas, and react in the ultraviolet light reaction box at 80°C for 40min to obtain intermediate A: 4-chloro-tetrahydrofuran-2-ethanol .

[0057] Add 1100g of intermediate A to another reaction device, and then add 800g of Grignard reagent R'MgCl, wherein R' is allyl; the reaction temperature is 35°C, and the reaction is stirred for 75min; the reaction is complete, post-treatment, and the intermediate Enzyme B: 4-allyl-tetrahydrofuran-2-ethanol.

[0058] Add 550g of intermediate B into a pressurized reaction device with a volume of 10L, and add 50g of sodium ethoxide as a catalyst, add 6000g of propylene oxide (PO), stir the reaction and control the reaction temperature to 175°C and the reaction pressure to 2.5 times the standard atmospheric pressure , The reaction time is 6.5h. After the reaction, the temperature was lowered to 50° C., and then an appropriate am...

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Abstract

The invention provides a synthesis method of unsaturated polyoxyethylene ether containing aerobic heterocyclic alkane. The synthesis method comprises the following steps: taking aerobic heterocyclic alkane with a terminal hydroxyl as a starting material, enabling the aerobic heterocyclic alkane and chlorine to have a chlorination reaction, enabling an obtained intermediate A and a Grignard reagent containing C2-C10 linear alkenyl to react to obtain an intermediate B, finally enabling the intermediate B and EO or / and PO to finish a polymerization reaction, and obtaining a target product. The invention further provides the unsaturated polyoxyethylene ether containing the aerobic heterocyclic alkane prepared through the synthesis method, the unsaturated polyoxyethylene ether containing the aerobic heterocyclic alkane can be used to prepare a polycarboxylate water reducer, so that the water reducing rate of the polycarboxylate water reducer is higher, the cement paste divergence is higher, and a better retarding effect is shown. The provided synthesis method and the unsaturated polyoxyethylene ether containing the aerobic heterocyclic alkane prepared through the synthesis method are suitable for large-scale industrial production, and have broad application prospects and market potentials.

Description

technical field [0001] The invention belongs to the technical field of concrete admixtures, in particular to a method for synthesizing unsaturated polyoxyethylene ether containing oxetane, and to the unsaturated polyoxyethylene containing oxetane prepared by the synthesis method. The ether also relates to the application of the unsaturated polyoxyethylene ether containing oxetane in the preparation of polycarboxylate water reducer. Background technique [0002] Polycarboxylate superplasticizer belongs to the third generation of building admixtures after lignosulfonate building admixtures and naphthalene-based building admixtures, and its water reducing rate and slump retention performance for precast concrete are significantly better than other types of building admixtures . The main reaction raw materials of commercially available polycarboxylate superplasticizers are: unsaturated carboxylic acid with copolymerization reactivity and unsaturated chain polymer with copolymer...

Claims

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Application Information

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IPC IPC(8): C08G65/28C08F283/06C08F220/06C04B24/26C04B103/30
CPCC04B24/2605C04B2103/302C08F283/065C08G65/2606C08F220/06
Inventor 朱伟亮
Owner SHANGHAI TAIJIE CHEM
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