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A kind of preparation method of high-performance grinding aid monomer diisopropanol monoethanolamine

A technology of monoethanolamine and diisopropanol, which is applied in the preparation of organic compounds, chemical instruments and methods, and the preparation of aminohydroxyl compounds, etc., can solve the problem of the small amount of the target product of diisopropanol monoethanolamine, monoethanolamine and propylene oxide Difficult to control the polymerization rate, poor material mass transfer, poor heat transfer effect, etc., to achieve the effect of reducing the generation of a large number of by-products, good control, and good heat transfer effect

Active Publication Date: 2016-04-06
杭州白浪助剂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The present invention provides a method for preparing high-performance grinding aid monomer diisopropanol monoethanolamine, which mainly solves the material mass transfer and heat transfer effects in the preparation of monomer diisopropanol monoethanolamine in the prior art Poor, the polymerization rate of monoethanolamine and propylene oxide is difficult to control, which will cause the generation of a large number of by-products, and the technical problems of the obtained diisopropanol monoethanolamine target product are less

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Example 1: The preparation method of a high-performance grinding aid monomer diisopropanol monoethanolamine of this example, the steps are:

[0017] Adopt 2M 3 Press external circulation spray polymerization equipment, 815kg propylene oxide (PO) monomer is prepared in the metering tank. Turn on the vacuum system, and suck 427kg ethanolamine and 210kg deionized water into the kettle. After the completion, the reaction kettle is closed after the nitrogen is discharged three times. Start the canned motor pump, open the steam valve of the heat exchanger, and slowly increase the temperature. When the temperature in the kettle rises to about 50°C, PO is slowly added dropwise, and the temperature rises significantly. When the temperature rises to 65°C, the cooling water is turned on and the material is smoothly fed. Polymerization process: 0.06Mpa≤P≤0.21Mpa, 60℃≤T≤75℃, after feeding, mature for 1.0hr, slightly open the reactor vacuum system, the vacuum degree is -0.035~-0.075MPa,...

Embodiment 2

[0018] Example 2: The preparation method of a high-performance grinding aid monomer diisopropanol monoethanolamine of this example, the steps are:

[0019] Adopt 2M 3 Press external circulation spray polymerization reaction equipment, 850kg propylene oxide (PO) monomer is prepared in the metering tank. Turn on the vacuum system, suck in 430kg of monoethanolamine and 230kg of deionized water into the kettle, and close the reactor after exhausting nitrogen three times. Start the canned motor pump, open the steam valve of the heat exchanger, and slowly increase the temperature. When the temperature in the kettle rises to 55℃, the PO is slowly added dropwise, the temperature rises obviously, the cooling water is turned on, and the feed is smoothly fed. The entire polymerization process: 0.05Mpa≤P ≤0.19Mpa, 55℃≤T≤75℃, after the feeding is finished, mature for 1.5hr, slightly open the vacuum system of the reactor, and the vacuum degree is -0.029~-0.070MPa, and the residual unreacted PO...

Embodiment 3

[0020] Example 3: The preparation method of a high-performance grinding aid monomer diisopropanol monoethanolamine of this example, the steps are:

[0021] Use 10M 3 Press external circulation spray polymerization equipment, 4250kg propylene oxide (PO) monomer is prepared in the metering tank. Turn on the vacuum system, suck in 2150kg of monoethanolamine and 1150kg of deionized water into the kettle, and close the reactor after exhausting nitrogen three times. Start the canned motor pump, open the steam valve of the heat exchanger, and slowly increase the temperature. When the temperature in the kettle rises to 50℃, start to slowly add PO, the temperature rises, turn on the cooling water, and smoothly feed the entire polymerization process: 0.07Mpa≤P≤ 0.23Mpa, 50°C≤T≤70°C, after the feeding is finished, mature for 1.5hr, slightly open the vacuum system of the reactor, the vacuum degree is -0.035~-0.073MPa, and remove the residual unreacted PO under reduced pressure. After finish...

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Abstract

The invention relates to a preparation method of a cement grinding aid raw material, in particular to a preparation method of high-performance grinding aid monomer diisopropanol monoethanolamine, and mainly aims to solve the technical problems of generation of a large quantity of byproducts, low yield of an obtained target product, namely, the diisopropanol monoethanolamine, and the like due to poor mass transfer and heat transfer effects of materials and difficulty in controlling the polymerization speed of monoethanolamine and epoxypropane during preparation of monomer diisopropanol monoethanolamine in the prior art. The preparation method comprises the following steps: preparing an epoxypropane monomer in a metering groove, starting a vacuum system, sucking the mononethanolamine and deionized water serving as a retarding agent into a polymerization reactor, discharging nitrogen, and closing the reactor repeatedly; and starting a shield pump, raising the temperature slowly, mixing the materials uniformly, starting to dropwise add the epoxypropane monomer slowly, introducing materials uniformly, fully curing at the end of material introduction, slightly opening the vacuum system of the reactor, removing the residual unreacted epoxypropane monomer under a reduced pressure, and cooling the materials to obtain a finished product.

Description

Technical field [0001] The invention relates to a method for preparing cement grinding aid raw materials, in particular to a method for preparing a high-performance grinding aid monomer diisopropanol monoethanolamine. Background technique [0002] Diisopropanol monoethanolamine product, as a green and environmentally friendly new cement grinding aid material, has an excellent grinding aid effect. It has good compatibility with triethanolamine, triisopropanolamine and other alcohols, amines and lipids. It can be used alone or in combination with other substances when making grinding aids. According to the characteristics of different cement materials, with diisopropanol monoethanolamine as the core raw material, after targeted compatibility, it can significantly improve the early and late strength of cement. The Chinese patent discloses a new method for preparing monoethanol diisopropanolamine (publication number: CN103435499A), which includes the following steps: weigh ethanolam...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C215/12C07C213/04
Inventor 赵冬友
Owner 杭州白浪助剂有限公司