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Dicarboxypolycaprolactone compound and its preparation method and application of inorganic filler dispersant

A technology of polycaprolactone and dicarboxylate, which is applied in the field of inorganic filler dispersant, application of inorganic filler dispersant, dicarboxypolycaprolactone compound and its preparation, can solve the problems of insufficient adsorption, slow adsorption speed and water content There are problems such as higher requirements, and the synthesis method is simple and efficient, the dispersion efficiency is improved, and the dispersion time is shortened.

Active Publication Date: 2021-06-11
YANTAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, synthetic polymer dispersants have a slow adsorption rate to inorganic particles, and the adsorption is not firm enough; polyvalent carboxylic acid dispersants tend to form a thin adsorption layer on the surface of inorganic particles, resulting in small steric hindrance, which is prone to flocculation. Dispersion stability is poor; coupling agent dispersants have disadvantages such as harsh use conditions, such as high requirements for the water content of the dispersed inorganic particles

Method used

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  • Dicarboxypolycaprolactone compound and its preparation method and application of inorganic filler dispersant
  • Dicarboxypolycaprolactone compound and its preparation method and application of inorganic filler dispersant
  • Dicarboxypolycaprolactone compound and its preparation method and application of inorganic filler dispersant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] A kind of synthetic method of dicarboxy polycaprolactone dispersant, comprises the following steps:

[0046] S1: Under a high-purity nitrogen atmosphere, put 3.426g (30mmol) ε-caprolactone and 0.324g (3mmol) benzyl alcohol into the reactor, add 12.2mg (0.03mmol) stannous octoate, and react at 130°C Obtain the polycaprolactone of monohydroxyl termination in 48 hours;

[0047] S2: Add 34.3g tetrahydrofuran to the product of step S1, stir to dissolve it into a homogeneous solution, add 0.353g (3.6mmol) maleic anhydride, add 0.183g (1.5mmol) of 4-dimethylaminopyridine and 40 ° C Next, react for 3 hours;

[0048] S3: Add 0.318 g (3 mmol) of 3-mercaptopropionic acid and 16.0 mg of azobisisobutyronitrile to the product obtained in step 2, and react at 60° C. for 48 hours. After the reaction finished, the reaction product was removed most of the solvent with a rotary evaporator, and then precipitated in a precipitant (methanol and ethanol mixture, the mass ratio of the two was ...

Embodiment 1

[0050] The product of embodiment 1 is mixed with tetrahydrofuran and the solution that mass concentration is 30% is dispersing aid, and dispersing aid is respectively mixed with epoxy resin (brand is E-51), unsaturated resin (commercial brand is 191), phenolic resin (the trade mark is 176), polyurethane resin, amino resin (trade name is 747) mix, and add-on is 0.5% of resin weight.

[0051] figure 2 It is the gel permeation chromatogram of Example 1. The number average molecular weight of the product is 15700g / mol (the peak molecular weight is 20994g / mol), and the molecular weight distribution is 1.66, indicating that the product is a high molecular weight polymer. When used as a dispersant, the adsorption of polycaprolactone molecules on the surface of inorganic particles can form a certain thickness of the adsorption layer (produce a large enough steric hindrance), which is conducive to maintaining the stability of dispersed inorganic particles.

[0052] Mixing photos of ...

Embodiment 2

[0056] A kind of synthetic method of dicarboxy polycaprolactone dispersant, comprises the following steps:

[0057] S1: Under a high-purity argon atmosphere, 9.131g (80mmol) ε-caprolactone and 0.163g (1.6mmol) n-hexanol were placed in the reactor, and 648mg (1.6mmol) of stannous octoate was added, at 100°C React for 4 hours to obtain monohydroxyl-terminated polycaprolactone;

[0058] S2: Add 9.3g 1,4-dioxane to the product of step S1, stir to make it dissolve into a homogeneous solution, add 0.157g (1.6mmol) maleic anhydride, in 19.5mg (0.16mmol) of 4- Dimethylaminopyridine and 10°C, reacted for 72 hours;

[0059] S3: Add 0.848 g (8 mmol) of 3-mercaptopropionic acid and 0.254 g (1.0 mmol) of azobisisoheptanonitrile to the product obtained in step 2, and react at 90° C. for 2 hours. After the reaction was finished, the reaction product was removed with a rotary evaporator to remove most of the solvent, and then precipitated in a precipitant (petroleum ether and ether mixture,...

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Abstract

The invention discloses a dicarboxy polycaprolactone compound, a preparation method thereof and an application of an inorganic filler dispersant. In the method, high-purity nitrogen or high-purity argon-protected ε-caprolactone and monohydric alcohol are placed in a reactor, a catalyst stannous octoate is added, and the reaction is carried out at 100-130° C. for 4-48 hours to obtain monohydroxyl-terminated Polycaprolactone; at 4-dimethylaminopyridine and 10-40°C, hydroxyl-containing polycaprolactone and maleic anhydride are esterified in solution; under the action of an initiator, the obtained product is regenerated React with 3-mercaptopropionic acid to obtain polycaprolactone with dicarboxyl groups at the end of the molecular chain. As a dispersant, the dicarboxypolycaprolactone compound prepared by the present invention can be quickly and firmly adsorbed on the surface of inorganic fillers, which not only meets the dispersion requirements of different inorganic filler particles, but also can significantly reduce the kinematic viscosity of the inorganic particle filling system, significantly improving The processing or construction performance of the system is improved.

Description

technical field [0001] The invention relates to an inorganic filler dispersant, which belongs to the field of functional materials, in particular to a dicarboxy polycaprolactone compound, a preparation method thereof and an application of the inorganic filler dispersant. Background technique [0002] Inorganic particles such as carbonates (e.g., calcium carbonate), sulfates (e.g., precipitated barium sulfate and calcium sulfate), silicates (e.g., kaolin, talcum powder, mica powder), etc. are widely used in plastics, rubber, coatings, etc. Fill modifier for materials. These inorganic particles have wide sources, low price, and good chemical stability. Adding them into plastics or coatings according to certain methods and proportions can not only reduce the cost of materials, but also improve the hardness, mechanical strength, wear resistance, Flame retardancy, etc., effectively improving the fluidity and processability of modified materials. However, the particle size of th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/91C08G63/08C08L67/06C08L61/20C08L63/00C08L61/06C08L75/04C08L67/04C08K9/10C08K3/26
CPCC08G63/08C08G63/912C08K2003/265C08L61/06C08L61/20C08L63/00C08L67/06C08L75/04C08L67/04C08K9/10C08K3/26
Inventor 郑耀臣高璇张新涛巩攀王立政王焕平李潮
Owner YANTAI UNIV
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