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Aminated polyether intermediate, preparation method and application

An intermediate and polyether technology, which is applied in the field of concrete admixture preparation, can solve the problems of uncontrollable side reactions of copolymerization reaction, uncontrollable molecular structure and weight average molecular weight of water reducer, easy chain transfer of phosphorus-containing groups, etc. , to achieve the effect of high reactivity

Inactive Publication Date: 2018-01-12
JIANGSU SOBUTE NEW MATERIALS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] The present invention aims to solve the problem that when unsaturated monomers containing phosphoric acid groups are introduced, the phosphorus-containing groups are prone to chain transfer, that is, the side reactions of the copolymerization reaction are uncontrollable, and the molecular structure and weight-average molecular weight of the obtained water reducer cannot be controlled. , provide a new synthetic route, introduce a new polymerization intermediate - aminated polyether intermediate, and use the aminated polyether intermediate to carry out phosphorous acid reaction to obtain a structure and weight average molecular weight controllable Products containing polyether side chains and phosphorous acid groups, and use them as water reducing agents

Method used

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  • Aminated polyether intermediate, preparation method and application
  • Aminated polyether intermediate, preparation method and application
  • Aminated polyether intermediate, preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0072] Preparation of polyether-based glycidyl ether M-1.

[0073] Weigh 1000 parts of methoxypolyether (M n =1000, b=18, c=3) into the reactor, then add 300 parts of solvent water, and then add 42 parts of NaOH. After stirring evenly, control the temperature of the reaction system between 30°C and 60°C, weigh 278 parts of epichlorohydrin and gradually add it to the above reaction system, and then weigh 2 parts of the catalyst tetrabutylammonium bromide and add it to the reaction system. After the addition, the reaction kettle was closed, and the temperature was raised to 80° C., and the reaction was continued for 20 h. After the reaction, under the condition of 60℃~80℃, distill off the volatile components under reduced pressure, including the unreacted epichlorohydrin and the reaction solvent water, to obtain a viscous light brown solid, and the reaction system was titrated by acid-base titration In the consumption of NaOH, the conversion rate of methoxy polyether is 99.4%....

Embodiment 2

[0082] Weigh 1952 parts of polyethyleneimine (a=45) as a primer, and heat up to 60-80°C. Weigh 15840 parts of M-1 and add 15840 parts of water to dilute, then gradually add to the reaction system. After the addition was completed, the temperature was raised to 100° C., and the reaction was continued for 5 h to obtain a tan liquid. Add 6 parts of phosphoric acid to neutralize excess NaOH.

[0083] Use room temperature cooling circulating water to cool the reaction system, under the condition of strong stirring, add 1952 parts of concentrated hydrochloric acid, add 2706 parts of phosphorous acid, and then gradually add 2676 parts of 37wt% formaldehyde, after the addition is completed, the temperature is raised to 100 ° C, and the reaction is continued for 20 hours to obtain Wine red liquid, tested by GPC, the weight average molecular weight is 19894, PDI=1.91.

Embodiment 3

[0085] Weigh 877 parts of polyethyleneimine (a=20) as a primer, and heat up to 60-80°C. Weigh 16448 parts of M-2 and dilute with 10965 parts of water, then gradually add to the reaction system. After the addition was completed, the temperature was raised to 80° C., and the reaction was continued for 12 hours to obtain a tan liquid. Add 12 parts of phosphoric acid to neutralize excess KOH.

[0086] Use room temperature cooling circulating water to cool the reaction system, under the condition of strong stirring, add 877 parts of concentrated sulfuric acid, add 1292 parts of phosphorous acid, then gradually add 37wt% formaldehyde 1338 parts, after the addition is completed, the temperature is raised to 110 ° C, and the reaction is continued for 15 hours to obtain Wine red liquid, tested by GPC, the weight average molecular weight is 18642, PDI=1.71.

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Abstract

The invention discloses an aminated polyether intermediate, a phosphorylation product utilizing the aminated polyether intermediate and application of the phosphorylation product as a water reducer. The aminated polyether intermediate is structurally characterized in that a main chain is formed by amine monomers, a side chain with certain steric hindrance and hydrophilic and hydrophobic propertiesis formed by polyether glycidyl ether, and meanwhile, newly-generated hydroxy groups are located on the side chain. A process for preparing the phosphorylation product from the aminated polyether intermediate is simple, and the obtained phosphorylation product can be used as the water reducer and has an excellent delayed coagulation effect and clay tolerance.

Description

technical field [0001] The invention belongs to the field of preparation of concrete admixtures, in particular to a preparation method and application of an aminated polyether intermediate and a phosphorylated product thereof. technical background [0002] Water reducer is a concrete admixture that reduces the amount of mixing water while keeping the slump of the concrete constant. Most of them are anionic surfactants, which can disperse cement particles after being added to concrete mixture, and can improve the working performance of concrete. [0003] With the development of industries such as ultra-long-span bridges, ultra-large-volume concrete, and super-high-rise buildings, higher requirements are placed on the strength and durability of concrete. Sulfonate water reducers such as water agents and naphthalene-based water reducers have been developed into a new generation of high-performance polycarboxylate water reducers. [0004] With the reduction of high-quality san...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G81/02C08F8/40C08F226/02C04B24/26C04B103/30
Inventor 冉千平王涛范士敏亓帅马建峰韩正王兵王衍伟刘加平
Owner JIANGSU SOBUTE NEW MATERIALS
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