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Aminated intermediate, and aminated polyether and phosphorylated star-like products, preparation method and application thereof

An intermediate and amination technology, applied in the field of amination intermediates, can solve the problems of uncontrollable molecular structure and weight-average molecular weight of superplasticizers, uncontrollable side reactions of copolymerization, and easy chain transfer of phosphorus-containing groups.

Active Publication Date: 2018-01-09
JIANGSU SOBUTE NEW MATERIALS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The present invention aims to solve the problem that when the 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. , to provide a new synthetic route, introduce a new polymerization intermediate - aminated intermediate, and then make it into an aminated polyether, and use the aminated polyether to carry out phosphorous acid reaction, without phosphorus-containing groups in the whole process Chain transfer effect, simple synthesis process, obtain a star-shaped product containing phosphorous acid group with controllable structure and weight average molecular weight, and use it as a cement dispersant

Method used

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  • Aminated intermediate, and aminated polyether and phosphorylated star-like products, preparation method and application thereof
  • Aminated intermediate, and aminated polyether and phosphorylated star-like products, preparation method and application thereof
  • Aminated intermediate, and aminated polyether and phosphorylated star-like products, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Preparation of Chlorinated Polyether M-1.

[0064] Weigh 1000 parts of methoxypolyether (M n =1000, d=18, e=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 the 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 99.1%. Similarly, the following chlorinated polyethers are prepared for the synthesis of aminated ...

Embodiment 2

[0072] Preparation of aminated intermediate N-1

[0073] Weigh 94 parts of phenol as a primer, gradually add 5853 parts of polyethyleneimine (a=45), stir evenly and then heat up to 60-80°C, weigh 162 parts of 37wt% formaldehyde, drop them completely within 2-4 hours, and then The temperature was raised to 85°C, and the reaction was kept for 6 hours. The obtained light brown liquid was tested by GPC, and the weight average molecular weight was 94+5853+14*3-6=5983, and the weight average molecular weight distribution was 1.78.

[0074] Similarly, the following aminated intermediates are prepared for the synthesis of aminated polyether intermediates.

[0075] N-2: 110 parts of hydroquinone, 3508 parts of polyethyleneimine (a=20), 389 parts of 37wt% formaldehyde, reaction temperature 95°C, reaction time 4h, light brown liquid, tested by GPC, weight average molecular weight It is 110+3508+14*4-8=3666, and the weight average molecular weight distribution is 1.75.

[0076] N-3: 10...

Embodiment 3

[0082] In a closed autoclave, use N-1 as the base, add 10833 parts of reaction solvent water, stir evenly, heat up to 60-80 °C, gradually add 30000 parts of chlorinated polyether M-1, then heat up to 100 °C, keep warm Reaction 8h.

[0083] After the reaction, cool down to 50°C-70°C, gradually add 5853 parts of catalyst concentrated hydrochloric acid, then add 9102 parts of phosphorous acid, and finally add 9000 parts of 37wt% formaldehyde, raise the temperature of the reaction to 100°C, and continue the heat preservation reaction for 30 hours to obtain reddish-brown Liquid, tested by GPC, the weight average molecular weight is 45352, PDI=3.41.

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Abstract

The invention discloses an aminated intermediate, and aminated polyether and phosphorylated star-like products, a preparation method and application thereof. The aminated intermediate is characterizedin that the aminated intermediate and the chlorinated polyether are subjected to amination reaction, so as to obtain the aminated polyether; the aminated polyether intermediate, phosphorous acid, a catalyst and aldehyde monomers are subjected to phosphorylation reaction, so as to obtain the star-like product containing phosphorous acid groups; the star-like product containing the phosphorous acidgroups can be used as a cement dispersant, and the better dispersing effect is realized.

Description

technical field [0001] The invention belongs to the field of preparation of concrete admixtures, in particular to an aminated intermediate, its aminated polyether and phosphorylated star product, a preparation method and an application. technical background [0002] As a commonly used concrete admixture, water reducing agent can effectively reduce the amount of concrete mixing water and improve the working performance of concrete. Since the first appearance of polycarboxylate water reducer in the 1980s, it has gradually replaced aliphatic sulfonate water reducer with its advantages of low dosage, high water reducing rate, good workability, and outstanding fluidity retention ability. High-efficiency water reducers such as melamine sulfonate-based water reducers and naphthalene-based sulfonate-based water reducers have been widely used in civil or engineering projects such as construction, railways, bridges, hydropower, and nuclear power. [0003] However, the polycarboxylate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G14/06C08G81/02C08F8/42C08F226/02C04B24/24C04B103/30C04B103/40
CPCC04B24/246C04B2103/408
Inventor 王涛冉千平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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