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A kind of phosphorous-containing acrylic resin polymer and preparation method thereof

An acrylic resin and polymer technology, applied in the fields of polymer materials and flame retardant materials, can solve the problems of negative effects on polymerization stability, cumbersome processes, easy formation of oligomers, etc. , the effect of mild reaction conditions

Active Publication Date: 2021-10-26
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But this method also has a series of problems: first, no polymerization inhibitor is added in the synthesis process of this phosphorus-containing monomer, and in the preparation process, it is easy to cause the monomer to self-polymerize and form oligomers easily, which also leads to It is understood that in the later stage of the polymer polymerization process, the increase in the amount of phosphorus-containing monomers will easily have a negative impact on the polymerization stability in the process; secondly, the prepared phosphorus-containing acrylic acid monomers are phosphoric acid monoesters, phosphoric acid diesters and pyrophosphates. Phosphoric acid and a mixture of unreacted hydroxyl monomers
The other by-product pyrophosphoric acid has strong acidity, which will cause other negative effects and affect the performance and application of the product
And if the mixture is further separated and purified, since the properties of these products are relatively close, the separation and purification steps are many and tedious, and a variety of organic reagents are used, which will cause cumbersome processes and greatly increase the cost, which is not conducive to industrial application.

Method used

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  • A kind of phosphorous-containing acrylic resin polymer and preparation method thereof
  • A kind of phosphorous-containing acrylic resin polymer and preparation method thereof
  • A kind of phosphorous-containing acrylic resin polymer and preparation method thereof

Examples

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Effect test

Embodiment 1

[0058] The preparation of the phosphorus-containing acrylic acid mixed monomer described in this example, the specific raw material composition is shown in Example 1 of Table 1, and is prepared by the following steps:

[0059] 1. Inhibitor, hydroxyacrylic acid monomer are added in the reaction kettle, stir evenly;

[0060] II. Add phosphorus pentoxide to the system of step I in four batches, and control the temperature of the system below 20°C during the process; after the addition of phosphorus pentoxide is completed, the system is heated to 80°C for 4 hours;

[0061] III. Add water to the reaction system obtained in step II, and control the suitable temperature to 85° C. for 1.5 h; the phosphorus-containing acrylic acid monomer mixture can be prepared.

[0062] The schematic diagram of the preparation mechanism of the phosphorous-containing acrylic acid monomer mixture is as follows: figure 1 As shown, the phosphoric acid monoester, phosphoric acid diester, pyrophosphoric a...

Embodiment 2

[0064] The preparation of the phosphorus-containing acrylic acid mixed monomer described in this example, the specific raw material composition is shown in Example 2 of Table 1, which is prepared through the same steps as Example 1, the difference is: reaction step II, phosphorus pentoxide The reaction temperature and time after the post-feeding are completed are 80°C and 3h respectively; the reaction temperature and time of step III are 90°C and 1h respectively;

[0065] The schematic diagram of the preparation mechanism of the phosphorous-containing acrylic acid monomer mixture is as follows: figure 1 As shown, the prepared phosphorus-containing acrylic acid monomer mixture is specifically composed of phosphoric acid monoester, phosphoric acid diester, phosphoric acid and unreacted hydroxyl acrylic monomer; As shown in Table 1.

Embodiment 3

[0067] The schematic diagram of the preparation mechanism of the phosphorous-containing acrylic acid monomer mixture is as follows: figure 1 As shown, the preparation of the phosphorus-containing acrylic acid mixed monomer described in this example, the specific raw material composition is shown in Example 2 of Table 1, and is prepared through the same steps as Example 1, the difference is that the reaction step II, pentoxide The reaction temperature and time after the addition of diphosphorus is completed are respectively 80°C and 3h; the reaction temperature and time of step III are respectively 80°C and 2h;

[0068] The prepared phosphorus-containing acrylic acid monomer mixture is specifically composed of phosphoric acid monoester, phosphoric acid diester, phosphoric acid and unreacted hydroxyl acrylic acid monomer; the ratio of phosphoric acid monoester, phosphoric acid diester, and phosphoric acid is determined by titration, and the results are shown in Table 1 shown.

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Abstract

The invention discloses a phosphorous-containing acrylic resin polymer and a preparation method thereof. The method includes: esterifying phosphorus pentoxide with hydroxyl-containing acrylic acid monomers, hydrolyzing, converting pyrophosphoric acid into phosphoric acid, converting most of phosphoric acid diesters into phosphoric acid monoesters, and obtaining phosphoric acid monoesters mainly composed of phosphoric acid monoesters. Phosphorus-containing acrylic monomer mixture composed of diester, phosphoric acid and unreacted hydroxyacrylic acid monomer as by-products; radical polymerization reaction is carried out by the phosphorus-containing acrylic monomer mixture, other acrylic monomers and epoxy resin under the action of an initiator , taking advantage of the fact that epoxy resin can undergo free radical graft polymerization with acrylic resin during the polymerization process, and at the same time, the epoxy group can undergo condensation reaction with phosphoric acid in the phosphorus-containing acrylic acid mixture, and the by-product phosphoric acid is introduced into the polymer molecular chain to prepare A phosphorous acrylic resin polymer with flame retardant properties. The invention also introduces the flame-retardant application of the phosphorous-containing acrylic resin polymer in materials such as cotton fabrics.

Description

technical field [0001] The invention belongs to the field of polymer materials and flame-retardant materials, and in particular relates to a phosphorous-containing acrylic resin polymer and a preparation method thereof. Background technique [0002] Acrylic resin has the advantages of excellent film-forming properties, weather resistance, easy construction and low price, so it is widely used in industries such as textiles, construction, coatings and papermaking. In recent years, with the improvement of people's safety awareness, many fields related to the application of acrylic emulsion, especially the fields of papermaking and textiles, have put forward flame retardant requirements. However, acrylic resin is a flammable polymer and has potential safety hazards, so it is necessary to carry out flame-retardant treatment on acrylic resin. There are two main flame retardant modification methods of acrylic resin: one is to add flame retardants. In order to achieve a better flam...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F283/10C08F230/02C08F220/06C08F220/18C08F220/32C08F220/14
CPCC08F283/10C08F230/02C08F220/06C08F220/1804C08F220/325C08F220/14C08F220/1808C08F220/1802
Inventor 胡健徐桂龙乔辉梁云王宜龙金曾靖山
Owner SOUTH CHINA UNIV OF TECH