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Preparation method and application of vinyl alcohol amine and polyether thereof

A technology of vinyl alcohol amine and vinyl alcohol, which is applied in the field of preparation of vinyl alcohol amine and its polyether, which can solve the problems of affecting the water reducing and slump retention effect of water reducing agent, limited early strength improvement, and affecting early strength effect, etc. , to achieve the effect of good slump retention and water reduction performance, excellent slump retention and water reduction function, and excellent polymerization activity

Pending Publication Date: 2022-07-29
河北凯瑞化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at the deficiencies of the prior art, the present invention provides a preparation method and application of vinyl alcohol amine and its polyether, which solves the problem that the electron cloud density of the introduced amide group is low, and the early strength is limited, and the amide group is due to Its adsorption effect on the cement surface is weaker than that of the carboxyl group, and its introduction will also affect the water-reducing and slump-preserving effect of the water-reducing agent itself; after the alcohol amine ester group is hydrolyzed in the alkaline environment of cement, it will be more free in the water phase, which is not conducive to its The contact with the cement surface will affect its early strength; the activity of the larger molecular weight polyether monomer is reduced, which puts forward higher requirements for the polymerization conditions and indirectly increases the problem of cost

Method used

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  • Preparation method and application of vinyl alcohol amine and polyether thereof
  • Preparation method and application of vinyl alcohol amine and polyether thereof
  • Preparation method and application of vinyl alcohol amine and polyether thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0037] A kind of preparation method of vinyl alcohol amine and polyether thereof, specifically comprises the following steps:

[0038] Step 1, crude product preparation: add 630.8g of diethanolamine to a stainless steel high-pressure reactor with a stirring device, seal the equipment, then replace with nitrogen and heat up, when the temperature reaches 150 ° C, feed acetylene gas and nitrogen into the reactor, wherein The volume of acetylene accounts for 70%, and the reaction pressure is controlled at 0.3Mpa. After reaching the reaction pressure, close the inlet valve to start the reaction. When the pressure drops to 0.15Mpa, continue to introduce acetylene and nitrogen. Repeat the above operation. During the change, the reaction was completed, and the total volume of the acetylene intake was 67 L at this time, the temperature was lowered to 60° C., the nitrogen was replaced to normal pressure, and the crude product of vinyldiethanolamine was obtained by discharging.

[0039] ...

Embodiment 2

[0043] A kind of preparation method of vinyl alcohol amine and polyether thereof, specifically comprises the following steps:

[0044] Step 1. Preparation of crude product: add 666g of diisopropanolamine to a stainless steel high-pressure reactor with a stirring device, seal the equipment, then replace with nitrogen and heat up, when the temperature reaches 130 ° C, feed acetylene gas and nitrogen into the reactor , in which the volume of acetylene accounts for 75%, and the reaction pressure is controlled at 0.4Mpa. After reaching the reaction pressure, close the inlet valve to start the reaction. When the pressure drops to 0.2Mpa, continue to introduce acetylene and nitrogen, and repeat the above operation. When the reaction pressure is 30min When there is no obvious change, the reaction is completed. At this time, the total intake volume of acetylene is 62 L. The temperature is lowered to 60° C., nitrogen is replaced to normal pressure, and the crude product of vinyldiisoprop...

Embodiment 3

[0049] A kind of preparation method of vinyl alcohol amine and polyether thereof, specifically comprises the following steps:

[0050] Step 1, crude product preparation: add 644g of dibutanolamine to a stainless steel high-pressure reactor with a stirring device, seal the device, then replace with nitrogen, and heat up, when the temperature reaches 170 ° C, feed acetylene gas and nitrogen into the reactor, Among them, the volume of acetylene accounts for 80%, and the reaction pressure is controlled at 0.5Mpa. After reaching the reaction pressure, the inlet valve is closed to start the reaction. When the pressure drops to 0.2Mpa, acetylene gas and nitrogen gas are continued to be introduced, and the above operation is repeated. When there is a significant change, the reaction is completed. At this time, the total intake volume of acetylene is 44 L. The temperature is lowered to 60° C., nitrogen is replaced to normal pressure, and the crude product of vinyldibutanolamine is obtai...

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Abstract

The invention discloses a preparation method and application of vinyl alcohol amine and polyether thereof. The preparation method specifically comprises the following steps: step 1, preparing a crude product; step 2, purification; and step 3, preparing polyether. The invention relates to the technical field of synthesis of concrete admixtures. According to the vinyl alcohol amine and the preparation method and application of the polyether thereof, on one hand, the vinyl alcohol amine structure increases the density of double-bond electron cloud and enhances the polymerization activity of double bonds due to the conjugation of the double bonds and nitrogen atoms, and on the other hand, due to the strong coordination effect of the nitrogen atoms, the early strength function can be better played, and the early strength performance of the polyether is improved. The double-tail structure provided by the vinyl alcohol amine can effectively improve the side chain density of the early-strength water reducing agent, and the early-strength water reducing agent mother liquor synthesized by the vinyl alcohol amine has a good early-strength function and also has good slump-retaining and water-reducing performance.

Description

technical field [0001] The invention relates to the technical field of concrete admixture synthesis, in particular to a preparation method and application of a vinyl alcohol amine and a polyether thereof. Background technique [0002] In recent years, with the rapid development of the domestic market of polyether macromonomers for superplasticizers, new types of differentiated and functionalized macromonomers have been launched, the most representative of which is the new monovinyl ether structure with monovinyl ether structure. such as 4-hydroxybutyl vinyl ether, diethylene glycol monovinyl ether, ethylene glycol monovinyl ether as initiators and ethylene oxide polymerized from VPEG and EPEG. This type of macromonomer has better polymerization activity than conventional monomers such as methylalkenyl alcohol polyoxyethylene ether (such as HPEG, TPEG) due to the conjugation effect of its double bond and oxygen. Therefore, the polycarboxylate superplasticizer synthesized fro...

Claims

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Application Information

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IPC IPC(8): C08G65/28C08F283/06C08F283/10C08F220/06C04B24/26C04B103/30
CPCC08G65/2624C08F283/065C08F283/10C04B24/2694C04B2103/302C08F220/06
Inventor 刘丙柱王卫星王文亮于连林李雪峰
Owner 河北凯瑞化工有限公司