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Low relative molecular weight anti-clay type phosphoric acid-based superplasticizer, its preparation method and use

A superplasticizer and molecular weight technology, applied in the field of concrete admixtures, can solve the problems of difficult process control, cumbersome operation steps, and unsatisfactory effects.

Active Publication Date: 2020-10-23
JIANGSU SOBUTE NEW MATERIALS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the preparation method of the above-mentioned type of water reducer is usually to prepare unsaturated monomers containing phosphoric acid groups first, and then copolymerized by free radical polymerization. There is a possibility that the structure and molecular weight of the water reducer may change. The structure and molecular weight cannot be accurately controlled, and the operation steps are cumbersome and the process control is difficult
[0009] The above-mentioned patent documents disclose different clay-resistant phosphoric acid-based superplasticizers, but the effect is not very satisfactory. At the same time, the preparation process is relatively complicated and the industrial conditions are harsh. It is necessary to develop a phosphoric acid-based superplasticizer with a more novel structure. The water agent can not only maintain the good working performance of the concrete, but also the preparation is simple and effective

Method used

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  • Low relative molecular weight anti-clay type phosphoric acid-based superplasticizer, its preparation method and use
  • Low relative molecular weight anti-clay type phosphoric acid-based superplasticizer, its preparation method and use
  • Low relative molecular weight anti-clay type phosphoric acid-based superplasticizer, its preparation method and use

Examples

Experimental program
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Embodiment 1

[0048] Branched polyether polyamine, the synthesis initiator is ethylenediamine, the polymerization monomer is ethylene oxide, and the catalyst NaH (60wt%) addition (in terms of 100% purity) is 0.8% of the amount of ethylenediamine . Weigh 0.1 mol (6.0 g) of ethylenediamine, 11.3 mol (497.2 g) of ethylene oxide, and 32 mg of catalyst NaH (60 wt %). Add the above-mentioned initiator ethylenediamine and catalyst into a closed reaction kettle, evacuate to -0.1MPa, feed 20g of ethylene oxide, raise the temperature to 110°C to initiate the reaction and continue to feed the remaining ethylene oxide, keep the temperature for the reaction After 1 h, the volatile matter was removed under reduced pressure, and the insoluble matter was removed by filtration to obtain a branched polyether polyamine intermediate.

[0049] Branched polyether polyamine intermediate alcohol hydroxyl group (0.4mol) / phosphorylation reagent molar ratio is 1:1.05, weigh 5.1g NKC-9 and 49.6g (0.42mol) 85% phospho...

Embodiment 2

[0051] For the branched polyether polyamine, the synthetic initiator is 1,3-propylenediamine, the polymerization monomer is ethylene oxide, and the amount of catalyst sodium hydroxide added is 1.5% of the amount of 1,3-propylenediamine. Weigh 0.1 mol (7.4 g) of 1,3-propylenediamine, 24.7 mol (1086.8 g) of ethylene oxide, and 60 mg of catalyst sodium hydroxide. Add the above-mentioned initiator 1,3-propylenediamine and catalyst into a closed reaction kettle, vacuumize to -0.1MPa, feed 20g of ethylene oxide, raise the temperature to 110°C to initiate the reaction and continue to feed the remaining ethylene oxide alkane, keep warm for 3 hours, remove volatile substances under reduced pressure, and remove insoluble substances by filtration to obtain a branched polyether polyamine intermediate.

[0052] Branched polyether polyamine intermediate alcoholic hydroxyl group (0.4mol) / phosphorylation reagent molar ratio is 1:1.05, weigh 10.9g Amberlyst-15 and 49.6g (0.42mol) 85% phosphori...

Embodiment 3

[0054] For the branched polyether polyamine, the synthetic initiator is 1,2-phenylenediamine, the polymerization monomer is propylene oxide, and the amount of catalyst Na added is 1.6% of the amount of 1,2-phenylenediamine. 0.1 mol (10.8 g) of 1,2-phenylenediamine, 17.5 mol (1016.4 g) of propylene oxide, and 37 mg of catalyst Na were weighed. Add the above-mentioned initiator 1,2-phenylenediamine and the catalyst into the closed reaction kettle, evacuate to -0.1MPa, pass in 20g of propylene oxide, raise the temperature to 110°C to initiate the reaction and continue to pass in the remaining propylene oxide, Keeping the reaction for 5 hours, removing volatile substances under reduced pressure, and removing insoluble substances by filtration to obtain a branched polyether polyamine intermediate.

[0055] Branched polyether polyamine intermediate alcoholic hydroxyl group (0.4mol) / phosphorylation reagent molar ratio is 1:1.1, weigh 20.5g NKC-9 and 82.1g (0.44mol) 76% polyphosphoric...

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Abstract

The invention provides a low-relative-molecular-weight anti-clay type phosphate-based superplasticizer, and a preparation method and application thereof. The low-relative-molecular-weight anti-clay type phosphate-based superplasticizer has excellent anti-clay performance. The preparation method is easy to operate, mild in reaction conditions, capable of realizing industrial production and free ofenvironmental pollution. The preparation method comprises the following steps: (1) with polyamine of a specific structure as a starting agent, carrying out a ring opening reaction on epoxyalkane, andthen carrying out purifying to obtain a branched polyether polyamine intermediate with a terminal hydroxyl group; and (2) phosphorylating the terminal hydroxyl group of the branched polyether polyamine, and then carrying out purifying to obtain the low-relative-molecular-weight anti-clay type phosphate-based superplasticizer. The low-relative-molecular-weight anti-clay type phosphate-based superplasticizer has a molecular weight of 5, 000 to 14, 000.

Description

technical field [0001] The invention relates to a low relative molecular weight clay-resistant phosphoric acid-based superplasticizer, its preparation method and application, and belongs to the technical field of concrete admixtures. Background technique [0002] With the vigorous development of my country's infrastructure construction, the number of highways, railways, large bridges, tunnels, large-scale water conservancy and hydropower projects, high-rise buildings, and underground projects currently under construction ranks first in the world. The development of these major projects are all closely related to concrete materials, and put forward higher requirements for the strength and durability of concrete. The addition of high-performance polymer dispersants to concrete is the most effective, economical, and easiest technical way to reduce cement consumption, increase the utilization rate of industrial waste residue, and achieve high durability and performance improveme...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/327C08G65/26C04B24/32
CPCC04B24/32C04B2103/0079C04B2103/302C04B2103/32C04B2103/408C08G65/2624C08G65/2627C08G65/327
Inventor 刘加平冉千平亓帅王涛马建峰范士敏舒鑫曹攀攀
Owner JIANGSU SOBUTE NEW MATERIALS
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