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A kind of preparation method of ester anti-mud and slump-preserving polycarboxylate water reducer

A slump-preserving polycarboxylate technology, which is applied in the field of concrete water-reducing agent, can solve the problems of lower compressive strength ratio, poor slump-preserving effect, and reduced strength of hardened concrete, so as to improve the mud resistance of the product and weaken the interpenetrating effect , Improve the effect of branch chain size

Active Publication Date: 2018-06-26
KZJ NEW MATERIALS GROUP CO LTD +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] A large number of engineering examples and studies have shown that, compared with naphthalene-based, melamine-based and sulfamic acid-based water-reducers, polycarboxylate-based water-reducers are more sensitive to the clay content of aggregates. The water-reducing and dispersing ability of the water-reducing agent is severely reduced, and the slump-preserving effect is poor, resulting in a decrease in the strength of the hardened concrete. Although it can be alleviated by increasing the amount of the water-reducing agent, it is easy to cause the concrete to set for a long time and reduce the compressive strength ratio. and other issues, and with the continuous development of polycarboxylate technology, the water reducing rate of polycarboxylate superplasticizers continues to increase, which also increases the sensitivity of polycarboxylate superplasticizers, especially when the aggregate mud content is high , with a greater impact

Method used

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  • A kind of preparation method of ester anti-mud and slump-preserving polycarboxylate water reducer
  • A kind of preparation method of ester anti-mud and slump-preserving polycarboxylate water reducer
  • A kind of preparation method of ester anti-mud and slump-preserving polycarboxylate water reducer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Preparation of unsaturated amphoteric quaternary phosphorus salt: Weigh a certain amount of triphenylphosphine and allyl bromide in a molar ratio of 1:1.0. Add 20g of triphenylphosphine and 30g of carbon tetrachloride into a 100mL three-necked flask, and stir magnetically to dissolve. After the dissolution is completed, 9.3 g of allyl bromide is added dropwise (1 drop / 5 seconds). During the dropwise addition, magnetic stirring is carried out, and the reaction temperature is kept at about 40° C. After a period of reaction, a yellow-brown precipitate will precipitate out. After 4 hours, the precipitated product was recrystallized with acetone, and the recrystallized product was dried in a vacuum oven at 80° C. to finally obtain a white powder, which was an unsaturated amphoteric quaternary phosphonium salt.

[0028] (2) Esterification reaction: in parts by weight, 100.00 parts of polyethylene glycol monomethyl ether with a molecular weight of 1000, 51.65 parts of meth...

Embodiment 2

[0031] (1) Preparation of unsaturated amphoteric quaternary phosphorus salt: Weigh a certain amount of triphenylphosphine and allyl bromide in a molar ratio of 1:1.2, add 20g of triphenylphosphine and 30g of carbon tetrachloride into 100mL three ports In the flask, stir magnetically to dissolve. After the dissolution is completed, 11.07 g of allyl bromide is added dropwise (1 drop / 4 seconds). During the dropwise addition, magnetic stirring is carried out, and the reaction temperature is maintained at 45° C. After a period of reaction, a yellow-brown precipitate will precipitate out. After 5 hours, the precipitated product was recrystallized with acetone, and the recrystallized product was dried in a vacuum oven at 80° C. to finally obtain a white powder, which was an unsaturated amphoteric quaternary phosphonium salt.

[0032] (2) Esterification reaction: in parts by weight, 120.00 parts of molecular weight are 1200 polyethylene glycol monomethyl ether, 43.05 parts of methacry...

Embodiment 3

[0035] (1) Preparation of unsaturated amphoteric quaternary phosphonium salt: Weigh a certain amount of triphenylphosphine and allyl bromide in a molar ratio of 1:1.3. Add 20g of triphenylphosphine and 30g of carbon tetrachloride into a 100mL three-necked flask, and stir magnetically to dissolve. After the dissolution is completed, 12 g of allyl bromide is added dropwise (1 drop / 3 seconds). During the dropwise addition, magnetic stirring is carried out, and the reaction temperature is maintained at about 48° C. After a period of reaction, yellowish-brown precipitates will precipitate out. After 6 hours, the precipitated product was recrystallized with acetone, and the recrystallized product was dried in a vacuum oven at 80° C. to finally obtain a white powder, which was an unsaturated amphoteric quaternary phosphonium salt.

[0036] (2) Esterification reaction: in parts by weight, 200.00 parts of molecular weight are 2000 polyethylene glycol monomethyl ether, 34.44 parts of ac...

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Abstract

The invention discloses a method for preparing ester soil-resistant and slump-retaining type polycarboxylic acid water reducing agents. The method includes steps of (1), carrying out reaction shown as a graph on triphenyl phosphine and allyl bromide in carbon tetrachloride according to a molar ratio of 1:1.0-1.5 to prepare unsaturated amphoteric quaternary phosphorus salt; (2), carrying out esterification reaction; (3), carrying out copolymerization reaction. The method has the advantages that the manufactured unsaturated amphoteric quaternary phosphorus salt is introduced into low-sensitivity soil-resistant type polycarboxylic acid water reducing agents in synthesis procedures, effects of inhibiting or reducing the activity of soil can be realized by side chains of cation groups of the quaternary phosphorus salt, accordingly, the water reducing agent adsorption of the soil can be reduced, effects of adsorbing and dispersing cement can be respectively realized by carboxylic acid radical ions and polyether side chains in molecular structures, and the ester soil-resistant and slump-retaining type polycarboxylic acid water reducing agents have soil-resistant adaptability.

Description

technical field [0001] The invention belongs to the technical field of concrete water reducers, and in particular relates to a preparation method of an ester anti-slump polycarboxylate water reducer. Background technique [0002] A large number of engineering examples and studies have shown that, compared with naphthalene-based, melamine-based and sulfamic acid-based water-reducers, polycarboxylate-based water-reducers are more sensitive to the clay content of aggregates. The water-reducing and dispersing ability of the water-reducing agent is severely reduced, and the slump-preserving effect is poor, resulting in a decrease in the strength of the hardened concrete. Although it can be alleviated by increasing the amount of the water-reducing agent, it is easy to cause the concrete to set for a long time and reduce the compressive strength ratio. and other issues, and with the continuous development of polycarboxylate technology, the water reducing rate of polycarboxylate sup...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F283/06C08F220/06C08F220/28C08F230/02C08F212/14C04B24/26C04B103/30
CPCC04B24/2694C04B2103/302C04B2103/308C08F283/065C08F220/281
Inventor 赖广兴方云辉赖华珍林艳梅林添兴
Owner KZJ NEW MATERIALS GROUP CO LTD
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