Preparation method of phosphono-group-containing water reducing agent

A phosphoric acid-based, superplasticizer technology, applied in the field of polycarboxylate superplasticizer preparation, can solve problems such as unstable product performance, and achieve the effect of improving steric hindrance effect and high adsorption density

Active Publication Date: 2017-11-10
JIANGSU SOBUTE NEW MATERIALS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] In order to solve the defects of the existing synthesis process of phosphoric acid-related water reducing agents, resulting in unstable product performance, the present invention provides a monomer structure with strong adjustability,

Method used

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  • Preparation method of phosphono-group-containing water reducing agent
  • Preparation method of phosphono-group-containing water reducing agent
  • Preparation method of phosphono-group-containing water reducing agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0081] Preparation of aminated polyether with a molecular weight of 354.

[0082] Chlorinated polyether preparation:

[0083] Initiator allyl alcohol, catalyst DMC. Weigh 100 parts of allyl alcohol and 1 part of catalyst DMC, put the above materials into the reactor, and vacuumize the reactor to -0.1MPa at room temperature. Then the temperature of the reaction kettle was raised to 100° C., and 20 parts of propylene oxide was passed into the reaction kettle. When the pressure in the reaction kettle dropped and the temperature rose, it indicated that the polymerization reaction started. When the pressure in the reactor no longer decreases, feed 338 parts of ethylene oxide into the reactor; when the pressure in the reactor no longer decreases, continue to feed 159 parts of epichlorohydrin into the reactor, and maintain the reactor during the feeding process. The temperature is between 110-130°C and the pressure is between 0.2-0.4MPa. After the feeding of epichlorohydrin is comp...

Embodiment 2

[0095] Preparation of aminated polyether with a molecular weight of 962.

[0096] Chlorinated polyether preparation:

[0097] Initiator 3-methyl-3-buten-1-ol, catalyst DMC. Weigh 100 parts of 3-methyl-3-buten-1-ol and 1.2 parts of catalyst DMC, put the above materials into the reactor, and vacuumize the reactor to -0.1MPa at room temperature. Then the temperature of the reaction kettle was raised to 100° C., and 20 parts of propylene oxide was passed into the reaction kettle. When the pressure in the reaction kettle dropped and the temperature rose, it indicated that the polymerization reaction started. Continue to feed 30 parts of propylene oxide, until the pressure of the reactor is no longer reduced, feed 782 parts of ethylene oxide into the reactor; 215 parts. During the feeding process, keep the temperature of the reactor between 110-130°C and the pressure between 0.2-0.4MPa. After the feeding of epichlorohydrin is completed, keep the temperature at 120°C for about 1h. ...

Embodiment 3

[0105] Phosphitylation of aminated polyethers.

[0106] Weigh 300 parts of aminated polyether M1 and add it into the reaction kettle. Under the cooling condition of circulating water, add 251 parts of acidic reagent 37% concentrated hydrochloric acid and 100 parts of reaction solvent water, then raise the temperature to 80°C, and add 210 parts of phosphorous acid . Weigh 206 parts of 37% formaldehyde aqueous solution and add them all into the reaction kettle within 30 minutes. Continue to fully stir at this temperature for 30 minutes, then raise the temperature to 100° C., the pressure in the reactor is 0.1 MPa, and the reaction time is 10 hours. After the reaction, the water and insoluble salts in the reaction system were removed by vacuum filtration and rectification device to obtain light brown unsaturated polyether monomer containing phosphorous acid group, denoted as N1(Q 1 OH=allyl alcohol, a:b=22:1, c=1, ethylenediamine is the aminating reagent). Tested by GPC, the m...

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Abstract

The invention discloses a phosphono-group-containing water reducing agent and a preparation method thereof. The phosphono-group-containing water reducing agent is in a comb-like structure, wherein the main chain has an acid anhydride group, carboxylate group or amido group; the main chain does not provide the initial water reducing capacity, but releases adsorption groups after being hydrolyzed under alkaline conditions in the later period, thereby enhancing the slump retaining capacity; side chains comprise pure polyether side chains and polyether side chains with an adsorption group at the terminal; the pure polyether side chains provide steric hindrance; and the adsorption groups comprise phosphono groups and phosphorous acid groups, and have multiple and centralized adsorption sites, thereby providing the initial adsorption capacity and dispersion capacity of the water reducing agent. The main adsorption groups in the phosphono-group-containing water reducing agent are phosphono groups; and carboxylates or acid anhydrides in the water reducing agent structure can continuously release new carboxyl adsorption groups through the reaction of water under alkaline conditions in the later adsorption period, thereby achieving better slump retaining properties.

Description

technical field [0001] The invention belongs to the field of preparation of concrete admixtures, in particular to a preparation method and application of a phosphoric acid group-containing polycarboxylate water reducer. Background technique [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. With the development of industries such as ultra-long-span bridges, ultra-large-volume concrete, and ultra-high-rise buildings, higher requirements are placed on the strength and durability of concrete. Sulfonate water reducers such as naphthalene-based water reducers have developed into a new generation of high-performance polycarboxylate water reducers. [0003] Since Nippon Shokubai first developed polycarboxylate superplasticizers in t...

Claims

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Application Information

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IPC IPC(8): C08F283/06C08F230/02C08F220/14C08F220/18C08F220/28C08F222/14C08F220/34C08F222/06C08F220/56C08F220/58C08F220/54C04B24/26C04B103/30
CPCC04B24/246C08F283/065C04B2103/30C08F220/281C08F220/34C08F222/14C08F220/1802C08F220/58
Inventor 王衍伟冉千平王涛亓帅范士敏马建峰杨勇刘加平
Owner JIANGSU SOBUTE NEW MATERIALS
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