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Double-branch allylamine polyethenoxy ether and synthetic method thereof

A branched chain allylamine polyoxyethylene ether, allylamine technology, applied in the field of double branched allylamine polyoxyethylene ether and synthesis, can solve the problem of rapid slump loss, limited development and poor adaptability and other problems, to achieve the effect of increasing the water removal step, high double bond retention rate, and reducing the content

Inactive Publication Date: 2014-04-30
SICHUAN SEDAR CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

With the continuous development of polycarboxylate superplasticizers, it also shows many shortcomings in its application, such as: polycarboxylate superplasticizers have poor adaptability to different substrates in different regions; they are highly sensitive to clay, and a small amount of clay exists It has a great influence on its water reduction effect; it is sensitive to temperature changes, especially in summer when the temperature is high and the slump loss is fast
These disadvantages of polycarboxylate superplasticizer limit its development and greatly restrict its regional use

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] In the present embodiment, double branched allylamine polyoxyethylene ether, its preparation method is as follows:

[0027] Use a 10L external circulation ethoxylation device. In the first step, add 250g of allylamine to the dry reactor, replace the air in the kettle with nitrogen for 3 times, turn on the external circulation to raise the temperature to 90°C, and start slowly adding ethylene oxide 405g, the reaction temperature is 95-100°C, the flow rate is controlled for 60 minutes, and the heat preservation and aging are 30 minutes. The second time, when the external circulation is started and the temperature rises to about 105°C, the heating and external circulation are stopped, and the water is removed by vacuuming. -115°C, the reaction pressure is less than 0.27Mpa, control the flow rate of epoxy for 4 hours, heat and age for 30 minutes, cool down to 100°C and vacuumize to remove low boiling point substances, and continue cooling to below 80°C to obtain a yellow vi...

Embodiment 2

[0029] In the present embodiment, double branched allylamine polyoxyethylene ether, its preparation method is as follows:

[0030] Use a 10L external circulation ethoxylation device. In the first step, add 250g of allylamine to the dry reactor, replace the air in the kettle with nitrogen for 3 times, turn on the external circulation to raise the temperature to 95°C, and start slowly adding ethylene oxide 405g, the reaction temperature is 100-105°C, the flow rate is controlled for 50min, and the heat preservation and aging are completed for 30min. The second time, when the external circulation is started and the temperature rises to about 105°C, the heating and external circulation are stopped, and the water is removed by vacuuming. After the water removal is completed, the external circulation is started and when the temperature rises above 110°C, 1996g of ethylene oxide is added, and the temperature is controlled at 110°C. -115°C, the reaction pressure is less than 0.27Mpa, c...

Embodiment 3

[0032] In the present embodiment, double branched allylamine polyoxyethylene ether, its preparation method is as follows:

[0033] Use a 10L external circulation ethoxylation device. In the first step, add 250g of allylamine to the dry reactor, replace the air in the kettle with nitrogen for 3 times, turn on the external circulation to raise the temperature to 110°C, and slowly add ethylene oxide 405g, the reaction temperature is 115-120°C, the flow rate is controlled for 40 minutes, and the heat preservation and aging are completed for 30 minutes. The second time, when the external circulation is started and the temperature rises to about 105°C, the heating and external circulation are stopped, and the water is removed by vacuumizing. -115°C, the reaction pressure is less than 0.27Mpa, control the epoxy flow rate for 3.5h to complete the addition, heat preservation and aging for 30min, cool down to 100°C and vacuumize to remove low boiling point substances, continue cooling t...

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Abstract

The invention discloses double-branch allylamine polyethenoxy ether and a synthetic method thereof. The double-branch allylamine polyethenoxy ether is synthesized from the following raw materials in mole ratio through two steps: allylamine and epoxyethane in a mole ratio of 1:(4-100), and a catalyst which accounts for 0.08-0.2% of the total mass of allylamine and epoxyethane. The double-branch allylamine polyethenoxy ether obtained by the method disclosed by the invention is high in double-bond retention rate under a reaction condition, and can be directly applied to synthesis of a polycarboxylate superplasticizer; and a two-step method is adopted, and a water removal step is increased, so that the content of a reaction byproduct namely polyethylene glycol is reduced.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, in particular to the field of polyether synthesis, in particular to a double branched allylamine polyoxyethylene ether and a synthesis method. Background technique [0002] Polycarboxylate superplasticizer is the third generation of high-efficiency water reducer developed in my country. At present, there are polyethylene glycol monomethyl ether (MPEG), allyl alcohol polyoxyethylene ether (APEG), isopentenol poly Several varieties such as oxyethylene ether (TPEG) and isobutyl alcohol polyoxyethylene ether (HPEG). With the continuous development of polycarboxylate superplasticizers, it also shows many shortcomings in its application, such as: polycarboxylate superplasticizers have poor adaptability to different substrates in different regions; they are highly sensitive to clay, and a small amount of clay exists It has a great influence on its water reduction effect; it is sensitive to te...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/26C07C217/08C07C213/04
Inventor 翟艳利王琦
Owner SICHUAN SEDAR CHEM
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