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Phosphorous flame-retardant water-based alkyd resin and preparation method thereof

A technology of water-based alkyd resin and phosphaphenanthrene, which is applied in the field of preparation of water-based alkyd resin and can solve problems such as complex technical processes

Inactive Publication Date: 2015-04-22
甘肃西北之光电缆有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Patent CN102604517A discloses a kind of waterborne alkyd resin coating, it is characterized in that, described waterborne alkyd resin coating is made by following steps: (a) under inert atmosphere, vegetable oil fatty acid, neopentyl glycol, isophthalic acid , Trimethylolpropane reacts under the effect of triphenyl phosphite to obtain oily alkyd resin; (b) under inert atmosphere, trimellitic anhydride and the described oily alkyd resin that step (a) make carry out esterification reaction to obtain an oily alkyd resin with an excess carboxyl group with an acid value of 40 to 70 mgKOH / g; (c) using a cosolvent to dilute the oily alkyd resin with an excess carboxyl group in step (b), adding neutralization neutralization degree is 80 to 100%, to obtain water-based alkyd resin; (d) take the water-based alkyd resin obtained in step (c) as base material, add water-based amino resin and solvent water, adjust with pH agent to adjust the pH value to 7.0 ~ 9.0 to prepare the water-based alkyd resin coating, the technical process is more complicated

Method used

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  • Phosphorous flame-retardant water-based alkyd resin and preparation method thereof
  • Phosphorous flame-retardant water-based alkyd resin and preparation method thereof
  • Phosphorous flame-retardant water-based alkyd resin and preparation method thereof

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preparation example Construction

[0022] The preparation steps of DOPOMA are:

[0023] In a three-neck flask equipped with a stirrer, a thermometer, and a reflux condenser, add a mixed solution of tetrahydrofuran and toluene of equal mass, DOPO and maleic anhydride are put in at a material ratio of 1:1.05, stir and heat, and the temperature is 84°C Backflow began to occur when the system was stable and reacted for 9 hours, and the color gradually deepened and turned green. After continuing to react for 24 hours, the color of the system was dark green. After 24 hours of heat preservation reaction, the reaction was stopped and cooled to room temperature. The system is layered, the lower layer is a dark green viscous liquid, and the upper layer is a light yellow clear liquid. The lower layer of viscous liquid is separated and washed with xylene for several times, then dried in an oven at 120°C for 48 hours, taken out and cooled to room temperature to obtain a light yellow Crystalline solid.

[0024] The preparat...

Embodiment 1

[0028] Add 51 parts of soy oil, 30 parts of trimethylolpropane, 20 parts of phthalic anhydride and 3 parts of xylene into a 100ml four-neck flask; blow nitrogen gas, start stirring, slowly raise the temperature, and heat to 180°C; at 160°C, there is a sound of oil splashing and reflux, and the system is a turbid liquid. After the temperature reaches 170°C, the system turns into a yellowish clear liquid after 20 minutes of reaction; Add 5.2 parts of DOPOMA in batches within the last 10 minutes; after the addition, slowly raise the temperature to 200°C for 30 minutes, and then slowly raise the temperature to 210°C; the final temperature of the heat preservation reaction is 210~220°C. As the reaction progresses, the color of the system gradually Deepen and finally turn orange-red; measure the acid value every half hour after the heat preservation reaction for 2 hours. When the temperature is 55mgKOH / g, stop heating, lower the temperature, and drain the xylene in the system; weigh...

Embodiment 2

[0030] Add 51 parts of soy oil, 28 parts of trimethylolpropane, 15 parts of phthalic anhydride and 3 parts of xylene into a 100 ml four-necked flask. Nitrogen was passed, stirring was started, and the temperature was raised slowly. (Heat to 180°C within 30~40min). At 160°C, there was a sound of oil splashing and backflow. The system is a cloudy liquid. After a temperature of 170°C, the reaction system turned into a slightly yellow clear liquid after 20 minutes of reaction. When the system temperature reaches 180°C, start to keep warm for 40 minutes. Add 11.2 copies of DOPOMA in batches within 10 minutes after the end of the heat preservation. After the feeding is completed, slowly raise the temperature to 200°C for 30 minutes, then slowly raise the temperature to 210°C, and the final temperature for the heat preservation reaction is 210~220°C (do not rapidly raise the temperature to 220°C to avoid bumping). As the reaction progressed, the color of the system graduall...

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Abstract

The invention relates to phosphorous flame-retardant water-based alkyd resin and a preparation method thereof. The phosphorous flame-retardant water-based alkyd resin comprises the following components in percentage by weight: 41.12%-45.78% of soya oil acid, 24.82%-26.77% of trimethylolpropane, 0%-17.48% of phthalic anhydride, 4.55%-11% of DOPOMA (2-[10-(9,10-dihydro-9-oxa-10-phosphaphenantrene-10-oxide-10-yl)] maleic acid), 3.67%-4.68% of trimellitic anhydride, 70%-85% of triethylamine calculated according to an acid value of a preliminary polymer, 7.46%-14.08% of propylene glycol n-butyl ether, 45%-70% of distilled water, and 2.62%-4.41% of a water-carrying agent. The preparation method comprises the steps that the raw material DOPOMA is synthesized by DOPO and MA at a molar ratio of 1:1.05; trimethylolpropane is blocked by soya oil acid to form dihydric alcohol with two functionality degrees; dihydric alcohol has an esterification reaction with phthalic anhydride to synthesize the alkyd resin; DOPOMA is added for polycondensation; trimellitic anhydride is added after an acid value of a system is appropriate; the preliminary polymer is formed; a triethylamine neutralizer is added after a solvent in the polymer is pumped; salt is formed; the distilled water is added finally; and the phosphorous flame-retardant water-based alkyd resin is formed.

Description

technical field [0001] The invention relates to the preparation technology of water-based alkyd resin. Background technique [0002] With the development of industry, the problem of environmental pollution is increasingly perplexing human beings, so the development of environmentally friendly coatings is an overall development trend. The fundamental way to solve the environmental pollution of coatings is to develop solvent-free coatings, water-based coatings, powder coatings and high-solid content coatings. Water-based paint is a new type of low-pollution, energy-saving, and resource-saving paint developed in the 1960s. Water-based coatings reduce environmental pollution because all or most of them replace organic solvents with water. With the strengthening of people's awareness of environmental protection and the high cost of organic solvents, water-based coatings have been paid more and more attention by people, and have been extensively researched and promoted. [0003...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/692C08G63/78
Inventor 郭军红陈碧碧杨保平崔锦峰周应萍李敏睿包雪梅魏小赟崔卓席满意李淑慧王心远
Owner 甘肃西北之光电缆有限公司
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