Polyether amine, preparation method of polycondensate containing phosphorous acid group and application of polycondensate as cement dispersing agent

A technology of aminated polyether and polycondensate, which is applied in the field of preparation of concrete admixtures, can solve problems such as uncontrollable side reactions of copolymerization reactions, easy chain transfer of phosphorus-containing groups, uncontrollable molecular structure and molecular weight of water reducers, etc. , to achieve the effect of convenient control

Active Publication Date: 2018-01-19
JIANGSU SOBUTE NEW MATERIALS +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] 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 molecular weight of the obtained water reducer cannot be controlled. It provides A new synthetic route, introducing a new polymerization intermediate - aminated polyether, and using the aminated polyether to carry out phosphorous acid reaction, to obtain a polycondensation type containing phosphorous acid group with controllable structure and molecular weight product, and use it as a cement dispersant

Method used

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  • Polyether amine, preparation method of polycondensate containing phosphorous acid group and application of polycondensate as cement dispersing agent
  • Polyether amine, preparation method of polycondensate containing phosphorous acid group and application of polycondensate as cement dispersing agent
  • Polyether amine, preparation method of polycondensate containing phosphorous acid group and application of polycondensate as cement dispersing agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Preparation of Chlorinated Polyether M-1.

[0063] Weigh 1000 parts of methoxypolyether (M n =1000, b=18, c=3) into the reactor, under the condition of -0.08MPa~-0.1MPa, vacuumize for 1h to remove water and a little volatile components in the polyether. Cool down to 40~60℃, in N 2 Under protection conditions, add SOCl to the above reaction system 2 155 parts, the temperature of the reaction system is controlled not to exceed 60°C during the dropwise addition. After the dropwise addition is completed, connect a cooling reflux device, raise the temperature of the reaction system to 80-90°C, continue the heat preservation reaction for 3-5 hours, and then distill out the acidic volatile components in the reaction system under reduced pressure to obtain a light brown product, which is passed through Liquid phase test showed that the yield of chlorinated polyether M-1 was 98.7%. Similarly, the following chlorinated polyethers were prepared for the synthesis of aminated p...

Embodiment 2

[0071] Preparation of Aminated Polyether N-1

[0072] Weigh 1952 parts of polyethyleneimine (a=45) as a primer, and heat up to 60-80°C. Weigh 1019 parts of M-1 and add 891 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 15 hours to obtain a wine-red liquid. The conversion rate of chlorinated polyether M-1 is close to 100% through liquid phase test.

[0073] Similarly, the following aminated polyether was prepared for the preparation of polycondensation monomers.

[0074]N-2: 877 parts of polyethyleneimine (a=20), 2221 parts of chlorinated polyether M-2, 1239 parts of solvent water, the reaction temperature is 120 °C, the reaction time is 10 h, the product is wine red liquid, and it is tested by liquid phase , the conversion rate of chlorinated polyether M-2 is close to 100%.

[0075] N-3: 275 parts of polyethylene polyamine (a=6), 3019 parts of c...

Embodiment 3

[0081] Weigh 94 parts of phenol as a primer, gradually add N-1 to the reaction system, stir evenly and then raise the temperature to 60-80°C. Weigh 81 parts of 37wt% formaldehyde, drop it completely within 2-4 hours, then raise the temperature to 85°C, and keep it warm for 6 hours.

[0082] After the reaction, turn on the circulating water at room temperature to cool, lower the temperature to 50-60°C, weigh 1952 parts of catalyst concentrated hydrochloric acid, gradually add to the above reaction system, then add 3772 parts of phosphorous acid, and finally add 3811 parts of 37wt% formaldehyde. The reaction temperature was raised to 100° C., and the reaction was continued for 10 h to obtain a reddish-brown liquid, which was tested by GPC with a molecular weight of 44497 and a PDI of 3.52.

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Abstract

The invention discloses polyether amine, a preparation method of a polycondensate containing a phosphorous acid group and application of the polycondensate as a cement dispersing agent. The polyetheramine has a polyether chain segment with steric hindrance property and hydrophilic-hydrophobic property, one end of the polyether chain segment is methoxyl-terminated while the other end of the polyether chain segment is amine monomer-terminated; the polyether chain segment is connected to a primary amino group N-H or a secondary amino group N-H of an amine monomer so as to present the characteristic of random grafting. Polycondensation reaction on a polycondensation monomer formed by grafting polyether amine on a benzene ring of a phenolic monomer and an aldehyde monomer as well as a phosphorous acid is carried out, so that a phosphite polycondensate is obtained; moreover, the polycondensate can be used as the cement dispersing agent, so that the polycondensate has a better dispersion effect.

Description

technical field [0001] The invention belongs to the field of preparation of concrete admixtures, in particular to an aminated polyether, a preparation method of its polycondensate containing phosphorous acid groups and its application as a cement dispersant. 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. 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] Compared with the sulfonate-based wat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G81/02C08G65/326C08G65/323C08G8/36C08G8/28C08G8/20C08G8/10C04B103/40
CPCC04B24/246C04B2103/408
Inventor 王衍伟范士敏亓帅王涛马建峰王兵韩正冉千平刘加平
Owner JIANGSU SOBUTE NEW MATERIALS
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