Cis-butenedioic acid di-2-ethylhexyl ester, method for synthesizing same and application of cis-butenedioic acid di-2-ethylhexyl ester to preparing polycarboxylic acid water reducing agents

A technology of maleic acid diester and maleic acid monoester, which is applied in the field of chemical synthesis, can solve problems such as poor slump retention performance, and achieve the effects of no safety hazard, good water solubility, and high yield

Inactive Publication Date: 2019-04-05
SICHUAN SEDAR CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The object of the present invention is to: in view of the problem that the above-mentioned existing polycarboxylate water reducers prepared by acrylates have poor slump performance, the present invention provides a maleic acid diester and its synthesis method, and its use in

Method used

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  • Cis-butenedioic acid di-2-ethylhexyl ester, method for synthesizing same and application of cis-butenedioic acid di-2-ethylhexyl ester to preparing polycarboxylic acid water reducing agents
  • Cis-butenedioic acid di-2-ethylhexyl ester, method for synthesizing same and application of cis-butenedioic acid di-2-ethylhexyl ester to preparing polycarboxylic acid water reducing agents
  • Cis-butenedioic acid di-2-ethylhexyl ester, method for synthesizing same and application of cis-butenedioic acid di-2-ethylhexyl ester to preparing polycarboxylic acid water reducing agents

Examples

Experimental program
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Effect test

Embodiment 1

[0036] A kind of synthetic method of maleic acid diester, comprises the following steps:

[0037] (1) Add 1000 parts of maleic anhydride and 469 parts of ethanol into the reaction kettle, raise the temperature to 60°C, stir for 3 hours, then raise the temperature to 90°C for 2 hours, after the reaction is completed, remove the unreacted ethanol by distillation under reduced pressure , to obtain maleic acid monoester;

[0038] (2) The gas in the reaction kettle is replaced with nitrogen by means of spray circulation, circulated for 1 minute, and 600 parts of maleic acid monoesters prepared in step (1) and 2.24 parts of sodium hydroxide are added successively, and nitrogen gas is carried out again. Replace and keep nitrogen circulation, then raise the temperature to 98°C, start adding ethylene oxide, stop when the pressure reaches 0.05mp, continue to add ethylene oxide when the pressure drops to 0.04mp, stop when the pressure reaches 0.1mp, After the pressure drops to 0.08mp, c...

Embodiment 2

[0040] A kind of synthetic method of maleic acid diester, comprises the following steps:

[0041] (1) Add 1000 parts of maleic anhydride and 1224.5 parts of diethylene glycol monomethyl ether into the reaction kettle, raise the temperature to 60°C, stir for 3 hours, then raise the temperature to 90°C for 2 hours, after the reaction is completed, reduce the pressure Distillation removes unreacted diethylene glycol monomethyl ether to obtain maleic acid monoester;

[0042](2) Nitrogen replacement is carried out by means of spray circulation, which is circulated for 1 minute, and 600 parts of maleic acid monoester prepared in step (1) and 4.05 parts of sodium ethoxide are successively added, nitrogen replacement is carried out again, and nitrogen circulation is maintained, Then heat up to 102°C, start adding propylene oxide, stop when the pressure reaches 0.05mp, continue to add propylene oxide when the pressure drops to 0.04mp, stop when the pressure reaches 0.1mp, and continue ...

Embodiment 3

[0044] A kind of synthetic method of maleic acid diester, comprises the following steps:

[0045] (1) Add 1000 parts of maleic anhydride and 612.2 parts of isopropanol into the reactor, raise the temperature to 60°C, stir for 3 hours, then raise the temperature to 90°C for 2 hours, after the reaction is completed, remove unreacted by vacuum distillation The isopropanol, obtain maleic acid monoester;

[0046] (2) Nitrogen replacement is carried out by means of spray circulation, and the circulation is 1 minute, followed by adding 600 parts of maleic acid monoester prepared in step (1) and 5.8 parts of sodium methoxide, nitrogen replacement is carried out again, and nitrogen circulation is maintained, Then heat up to 98°C, start adding propylene oxide, stop when the pressure reaches 0.05mp, continue to add propylene oxide when the pressure drops to 0.04mp, stop when the pressure reaches 0.1mp, and continue adding when the pressure drops to 0.08mp Propylene oxide, stop when the ...

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Abstract

The invention discloses cis-butenedioic acid di-2-ethylhexyl ester, a method for synthesizing the same and application of the cis-butenedioic acid di-2-ethylhexyl ester to preparing polycarboxylic acid water reducing agents. The cis-butenedioic acid di-2-ethylhexyl ester, the method and the application have the advantages that maleic acid monoester is generated from maleic anhydride by means of alcoholysis, then the maleic acid monoester is polymerized with ethylene oxide or propylene epoxide and is polymerized with ethylene oxide to generate novel diester which is the cis-butenedioic acid di-2-ethylhexyl ester, acrylate can be substituted with the cis-butenedioic acid di-2-ethylhexyl ester for preparing the polycarboxylic acid water reducing agents, accordingly, the slump retention performance of the polycarboxylic acid water reducing agents can be improved, and low slump loss of premixed concrete in two hours can be guaranteed; integral reaction, structures and molecular weights canbe controlled, the reaction can be smoothly and steadily carried out, water production can be prevented, the cis-butenedioic acid di-2-ethylhexyl ester is green and environmentally friendly and is high in yield, preparation procedures are simple, and industrial production can be facilitated. A structural formula of the cis-butenedioic acid di-2-ethylhexyl ester is shown. An R in the structural formula represents methyl or ethyl or propyl or isopropyl or normal-butyl or diethylene glycol mono-methyl ether, an m and an n in the structural formula are integers, the m ranges from 0 to 8, and the nranges from 1 to 15.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, in particular to a maleic acid diester and its synthesis method, and its application in the preparation of polycarboxylate water reducers. Background technique [0002] Polycarboxylate superplasticizer has become the core component of concrete admixture because of its low dosage, high water reducing rate, small slump loss, good cement adaptability, strong molecular structure adjustability, and environmental protection. In order to achieve long-term slump retention capacity, polycarboxylate superplasticizers usually introduce ester groups such as hydroxyethyl acrylate and hydroxypropyl acrylate into the main chain of the molecule, and use the gradual esterification of concrete under alkaline conditions to achieve The purpose of continuous adsorption and continuous dispersion, but acrylates are easy to self-polymerize and have poor stability. At the same time, the release rate of monoest...

Claims

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Application Information

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IPC IPC(8): C07C69/60C07C67/26C07C67/29C07C69/73C07C67/08C08F283/06C08F220/06C08G65/26C04B24/26C04B103/30
CPCC04B24/2694C04B2103/302C07C67/08C07C67/26C07C67/29C08F283/065C07C69/73C07C69/60C08F220/06
Inventor 杨俊范青松董振鹏于学龙
Owner SICHUAN SEDAR CHEM
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