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Preparation method of organic zinc or copper acrylic resin

A kind of technology of acrylic resin and acrylic acid, which is applied in paints, coatings, anti-fouling/underwater coatings containing biocide, etc. It can solve the problems of synthesis, high reaction temperature and complex synthesis process, and achieve low energy consumption and high reaction temperature The effect of low cost and simple process

Active Publication Date: 2018-01-05
BC P INC CHINA NAT PETROLEUM CORP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, patent document CN1544488A describes a kind of synthetic method of this type of resin, at first synthesize the basic salt of zinc or copper of organic acid, then synthesize the acrylic resin containing carboxyl group, make the basic salt of zinc or copper of organic acid and Carboxyl-containing acrylic resin reacts to produce zinc acrylate. The disadvantage is that the synthesis process is complicated, and acrylic acid prepolymer needs to be synthesized, and the reaction temperature is high.

Method used

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  • Preparation method of organic zinc or copper acrylic resin
  • Preparation method of organic zinc or copper acrylic resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Add 72g of acrylic acid, 99g of zinc hydroxide, 124g of sodium benzoate and 600g of solvent into a three-neck round bottom flask equipped with a stirrer, a thermometer, and an oil-water separator, stir, react at 80°C for 1.5h, and heat up to 110°C , after dehydration until no water is distilled off, the reaction obtains solution A containing organic zinc acrylate shown in structural formula I, X 2 is a zinc atom, the solvent is a mixture of xylene and n-butanol with a mass ratio of 4.9:1, and the total amount of distilled water is 18g;

[0023] (2) 84g methyl methacrylate, 62g butyl acrylate, 6.14g azobisisobutyronitrile and 2.05g tert-dodecyl mercaptan are mixed uniformly to obtain solution B, which is added to a constant pressure dropping funnel, and the step (1) The temperature of the obtained solution A is raised to 75°C, and the solution B in the constant pressure dropping funnel is dropped drop by drop within 2 hours under stirring at a rotating speed of 100r / ...

Embodiment 2

[0025] (1) Add 72g of acrylic acid, 98g of copper hydroxide, 122g of sodium benzoate and 600g of solvent into a three-neck round bottom flask equipped with a stirrer, a thermometer, and an oil-water separator, stir, react at 81°C for 1.4h, and heat up to 110°C , after dehydration until no water is distilled off, the reaction obtains solution A containing organic zinc acrylate shown in structural formula I, X 2 is a copper atom, the solvent is a mixture of xylene and n-butanol with a mass ratio of 5:1, and the total amount of distilled water is 18g;

[0026] (2) 83g methyl methacrylate, 63g butyl acrylate, 6.12g azobisisobutyronitrile and 2.04g tert-dodecyl mercaptan are mixed uniformly to obtain solution B, which is added to a constant pressure dropping funnel, and the step (1) The temperature of the obtained solution A was raised to 75°C, and under stirring at 100r / min, the solution B in the constant pressure dropping funnel was dropped drop by drop within 2 hours, kept warm,...

Embodiment 3

[0028] (1) Add 72g of acrylic acid, 98g of copper hydroxide, 117g of sodium benzoate and 600g of solvent into a three-necked round-bottomed flask equipped with a stirrer, a thermometer, and an oil-water separator, stir, react at 79°C for 1.6h, and heat up to 110°C , after dehydration until no water is distilled off, the reaction obtains solution A containing organic zinc acrylate shown in structural formula I, X 2 is a copper atom, the solvent is a mixture of xylene and n-butanol with a mass ratio of 5:1, and the total amount of distilled water is 18g;

[0029] (2) 85g methyl methacrylate, 68.2g butyl acrylate, 6.13g azobisisobutyronitrile and 2.04g tert-dodecyl mercaptan are mixed uniformly to obtain solution B, add a constant pressure dropping funnel, and Solution A obtained in step (1) was heated to 75°C, and under stirring at a speed of 100r / min, the solution B in the constant pressure dropping funnel was dropped dropwise within 2 hours, kept warm, and polymerized for 1 ho...

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Abstract

The invention provides a preparation method of acrylic resin containing organic zinc or copper. The method comprises the following steps: (1) making acrylic acid, zinc hydroxide / copper hydroxide, and sodium benzoate carry out reactions for 1 to 2 hours at a temperature of 78 to 82 DEG C, then heating the reaction product, dehydrating the reaction product until no water is distilled out to obtain an organic zinc / copper acrylate solution (A); (2) evenly mixing methyl methacrylate, butyl acrylate, azodiisobutyronitrile, and tert-dodecyl mercaptan, dropwise adding the solution (A) within 2 to 2.5 hours at a temperature of 74 to 76 DEG C under a rotation speed of 98 to 102 r / min, and maintaining the temperature to carry out polymerization reactions for 1 to 1.5 hours to obtain a acrylic resin solution containing organic zinc / copper, wherein the mole ratio of methyl methacrylate to butyl acrylate to acrylic acid, which is taken as the raw material in the step (1), is (0.8-0.9):(0.4-0.6):1. The preparation method has the advantages of simple technology, low reaction temperature, short time, little energy consumption, and easy control.

Description

technical field [0001] The invention relates to a preparation method of an organic zinc or copper-containing acrylic resin. Background technique [0002] Animals, algae, bacteria and fungi in the ocean can adhere to the bottom of ships, offshore platforms and other facilities submerged in seawater for a long time, forming marine biofouling, causing equipment damage or excessive energy consumption. Tin-free self-polishing antifouling coatings can effectively prevent marine biofouling, and its film-forming material is mainly acrylic resin containing zinc or copper. For example, patent document CN1544488A describes a kind of synthetic method of this type of resin, at first synthesize the basic salt of zinc or copper of organic acid, then synthesize the acrylic resin containing carboxyl group, make the basic salt of zinc or copper of organic acid and The carboxyl-containing acrylic resin reacts to generate zinc acrylate, but its disadvantage is that the synthesis process is com...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F222/02C08F220/14C08F220/18C09D135/00C09D5/16
Inventor 刘浩亮郭晓军段绍明张静张其滨
Owner BC P INC CHINA NAT PETROLEUM CORP
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