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Monoester phosphate containing meth-acrylate structure, its preparing method and use

A technology of methacrylate and methacrylic acid, applied in the direction of phosphorus organic compounds, chemical instruments and methods, dissolution, etc., can solve the problems of affecting the performance of the coating film, consuming large emulsifiers, etc., and achieve good performance and easy control of conditions , the effect of mild reaction conditions

Inactive Publication Date: 2007-03-21
SOUTH CHINA NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These surface-active monomers consume a large amount of emulsifiers in the preparation of microemulsions, which directly affects the performance of the coating film

Method used

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  • Monoester phosphate containing meth-acrylate structure, its preparing method and use
  • Monoester phosphate containing meth-acrylate structure, its preparing method and use
  • Monoester phosphate containing meth-acrylate structure, its preparing method and use

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Preparation of methacrylic acid-ω-hydroxydecyl ester: use 1.00 molar parts of methacrylic acid and 1.2 molar parts of 1,10-decanediol as raw materials to prepare monoester; catalyst p-toluenesulfonic acid accounts for methacrylic acid and 1 , 10% of the total mass of 10-decanediol, the polymerization inhibitor hydroquinone accounts for 0.1% of the total mass of methacrylic acid and 1,10-decanediol, the reaction condition is 75°C, and the reaction time is 6h;

[0026] (2) Preparation of phosphorylation reagent: take 0.0293 mole parts of phosphoric acid with a mass fraction of 85%, add 0.0288 mole parts of phosphorus pentoxide in batches under stirring, stir and heat up to 88°C for 1 hour after the addition, and prepare poly Phosphoric acid serves as a phosphorylation reagent. Let cool and set aside.

[0027] (3) Phosphorylation reaction: get 0.02 mole portion of monoester obtained in step (1) and the newly prepared whole phosphorylation reagent in step (2) to react ...

Embodiment 2

[0030] (1) Preparation of methacrylic acid-ω-hydroxydecyl ester: prepare monoester with 1.00 molar parts of methacrylic acid and 1.25 molar parts of 1,10-decanediol; catalyst p-toluenesulfonic acid accounts for methacrylic acid and 1 , 12% of the total mass of 10-decanediol, the polymerization inhibitor hydroquinone accounts for 0.15% of the total mass of methacrylic acid and 1,10-decanediol, the reaction conditions are 78 ° C, and the reaction time is 5h;

[0031] (2) Preparation of phosphorylation reagent: Take 0.0293 mole parts of phosphoric acid with a mass fraction of 85%, add 0.0282 mole parts of phosphorus pentoxide in batches under stirring, stir and heat up to 89°C for 1.5h after the addition, and obtain more Polyphosphoric acid was used as a phosphorylation reagent. Let cool and set aside.

[0032] (3) Phosphorylation reaction: get monoester 0.02 mole portion obtained in step (1) and the newly prepared phosphorylation reagent reaction in step (2) to prepare phosphor...

Embodiment 3

[0035] (1) Preparation of methacrylic acid-ω-hydroxydecyl ester: prepare monoester with 1.00 molar parts of methacrylic acid and 1.3 molar parts of 1,10-decanediol as raw material; catalyst p-toluenesulfonic acid accounts for methacrylic acid and 1 , 11% of the total mass of 10-decanediol, the polymerization inhibitor hydroquinone accounts for 0.15% of the total mass of methacrylic acid and 1,10-decanediol, the reaction conditions are 80°C, and the reaction time is 5h;

[0036] (2) Preparation of phosphorylation reagent: Take 0.0293 mole parts of phosphoric acid with a mass fraction of 85%, add 0.0285 mole parts of phosphorus pentoxide in batches under stirring, stir and heat up to 90°C for 1.2h after the addition, and obtain more Polyphosphoric acid was used as a phosphorylation reagent. Let cool and set aside.

[0037] (3) Phosphorylation reaction: get 0.02 mole parts of the monoester obtained in step (1) and react with the newly prepared phosphorylation reagent in step (2)...

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Abstract

The monoester phosphate containing methyl acrylate structure has also 1, 10-decamethyleneglycol and phosphate structure in its molecule. The preparation process of the monoester phosphate includes preparing monoester with methyl acrylic acid and 1, 10-decamethyleneglycol, preparing monoester phosphate with the monoester and phosphating reagent, saponifying the monoester phosphate to produce salt type monoester phosphate, and other steps. The product has high emulsifying performance and high reaction activity, and may be used as surfactant monomer for preparing micro emulsion paint, assistant, etc. The preparation process has mild reaction condition, high monoester yield and no need of solvent.

Description

(1) Technical field [0001] The invention relates to a phosphoric acid monoester containing a methacrylate structure, a preparation method thereof and its application as a surface active monomer, and belongs to the technical field of chemical engineering. (2) Background technology [0002] It is a common feature of surfactants to contain a hydrophilic structure (polar structure) on one side and an lipophilic structure (non-polar structure) on the other. For surface-active monomers (surfactants with carbon-carbon double bonds), existing reports are mostly surfactants containing sulfonic acid polar groups, such as Tang Guangliang et al. Surface-active monomers (Acta Polymer Sinica, 2000, 3: 267-270) prepared by chloropropane and sodium sulfite; , 4-TDI), maleic anhydride (MA), 2-hydroxyethyl methacrylate (2-HEMA), surface-active monomer prepared by sodium sulfite (Journal of South China Normal University, 2003, 2: 76-80 ). These surface-active monomers co...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/09B01F17/14C09K23/14
Inventor 李国明石艳红
Owner SOUTH CHINA NORMAL UNIVERSITY
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