Catalyst for preparing polycarboxylate water reducing agent macromonomer and preparation method thereof

A technology of polycarboxylate and macromonomer, which is applied in the field of catalyst for preparing polycarboxylate superplasticizer macromonomer and its preparation field, can solve the problems such as reduction and cannot be completely removed, and achieve the effect of improving purity

Inactive Publication Date: 2012-06-20
山西山大合盛新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] ③ sodium alkoxide as catalyst, such as sodium methoxide, sodium ethoxide, etc., all react with initiator methallyl alcohol or 3-methyl-3-butene-1-alcohol to generate methanol, ethanol, etc., and their boiling points are It is lower than the boiling point of water, so it cannot be completely removed during alkoxylation, and they react with alkylene oxide ring-opening to form impurity by-product polyether, reducing methallyl polyoxyalkylenyl ether and isoprenyl polyethers. Purity of oxyalkylene ethers

Method used

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  • Catalyst for preparing polycarboxylate water reducing agent macromonomer and preparation method thereof
  • Catalyst for preparing polycarboxylate water reducing agent macromonomer and preparation method thereof
  • Catalyst for preparing polycarboxylate water reducing agent macromonomer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Put 40kg of methallyl alcohol into a 100L reaction kettle, cut 0.8kg of sodium metal into small pieces and put it into the feeding device, pass nitrogen to replace the air in the reaction kettle, keep the vent valve open and pass nitrogen, and the condenser Pass in cooling water, open the feeding device, and feed 0.16kg once every 10 minutes. Control the temperature of the reaction system not to exceed 120°C. Close the feeding valve after adding the metal sodium, and continue the reaction until the reaction liquid has no bubbles. The mass percent concentration of sodium methallylate in the obtained methallyl alcohol solution of sodium methallylate was 8%.

[0028] Add 348g of the above catalyst into 2.0kg of methallyl alcohol, drop into a 50L autoclave while stirring, feed N 2 Replace three times, raise the temperature to 100°C, introduce 1.7kg of ethylene oxide, raise the temperature to 160°C, react for about 30 minutes, continue to add 13.0kg of ethylene oxide, keep t...

Embodiment 2

[0032] Put 40kg of 3-methyl-3-butene-1-alcohol into a 100L reactor, cut 1.6kg of sodium metal into small pieces and put it into the feeding device, feed nitrogen to replace the air in the reactor, keep the vent valve open and Introduce nitrogen, feed cooling water into the condenser, open the feeding device, feed once every 10 minutes, 0.16kg each time, control the temperature of the reaction system not to exceed 120°C, close the feed valve after adding metal sodium, and continue the reaction until no bubbles are generated in the reaction solution. The mass percent concentration of 3-methyl-3-butene-1-alcohol sodium in the 3-methyl-3-butene-1-alcohol solution of gained 3-methyl-3-butene-1-alcohol sodium 18%.

[0033] Add 174g of the above catalyst into 2.0kg of 3-methyl-3-buten-1-alcohol, drop it into a 50L autoclave while stirring, and feed N 2 Replace three times, raise the temperature to 100°C, introduce 2.0kg of ethylene oxide, raise the temperature to 160°C, react for a...

Embodiment 3

[0037] Put 40kg of methallyl alcohol into a 100L reactor, cut 1.6kg of sodium metal into small pieces and put it into the feeding device, feed nitrogen to replace the air in the reactor, keep the vent valve open and feed nitrogen, and put the condenser Put in cooling water, open the feeding device, feed once every 10 minutes, 0.16kg once, control the temperature of the reaction system not to exceed 120°C, close the feeding valve after adding the metal sodium, and continue the reaction until the reaction liquid has no bubbles. The mass percent concentration of sodium methallylate in the resulting methallyl alcohol solution of sodium methallylate was 16%.

[0038] Add 174g of the above catalyst into 2.0kg of methallyl alcohol, drop into a 100L autoclave while stirring, feed N 2Substitute three times, raise the temperature to 100°C, introduce 5kg of ethylene oxide, raise the temperature to 160°C, react for about 30min, continue to add 56.1kg of ethylene oxide, keep the reaction t...

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Abstract

The invention discloses a catalyst for preparing a polycarboxylate water reducing agent macromonomer, which is a methallyl alcohol solution of sodium methallyl alcohol or a 3-methyl-3-butene-1-alcoholic solution of 3-methyl-3-butene-1-sodium alcoholate; and the solution contains 5-20 percent by mass of sodium methallyl alcohol or 3-methyl-3-butene-1-sodium alcoholate. The preparation method comprises the following steps of: putting methallyl alcohol or 3- methyl-3-butene-1-sodium alcoholate into a reaction kettle, cutting sodium metal into small blocks, and adding into a feeding device; keeping an emptying valve in an open state and introducing nitrogen; and adding metal sodium in batch, controlling the temperature of a reaction system not to surpass 120 DEG C, closing a feed valve after the metal sodium is added, continually reacting till a reaction liquid does not produce air bubbles, closing the emptying valve, stopping introducing nitrogen, and discharging. Due to the adoption of the catalyst, byproducts are not generated in the preparation process of macromonomer methylallyl polyoxyethylene ether and prenyl polyoxyethylene ether, and the purity of the macromonomer can be effectively increased.

Description

technical field [0001] The invention relates to a catalyst, in particular to a catalyst for preparing a polycarboxylate superplasticizer macromonomer and a preparation method thereof. Background technique [0002] Methallyl polyoxyalkylene ether and isoprenyl polyoxyalkylene ether are the main raw materials for the production of polyether polycarboxylate high-performance water reducers. The polyether has good water solubility, No hydrolysis and deterioration, the synthetic water-reducing agent has high water-reducing rate, good reinforcement effect, does not corrode steel bars, and is environmentally friendly, so it can produce methallyl polyoxyalkylene ether and isoprene with high double bond activity Polyoxyalkylene ethers are very important. Domestic manufacturers of polyether raw materials mainly produce through anionic ring-opening polymerization of alkylene oxide, and most manufacturers use catalysts that more or less bring in impurities during the polymerization proc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28C07C29/70C07C33/03C07C33/025
Inventor 李军平王正波裴继凯赵婷婷刘学明王自卫
Owner 山西山大合盛新材料股份有限公司
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