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A kind of polycyclic carbonate resin and its rapid preparation method and application under normal pressure

A technology of carbonate resin and hydroxycyclic carbonate, which is applied in the field of carbonate resin, can solve the problems of easily mixed with impurities, unsatisfactory purity, increase reaction rate, etc., and achieve shortened reaction time, superior mechanical properties, and reduced toxicity Effect

Active Publication Date: 2020-08-18
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, in order to ensure the conversion rate of the product per unit time, this step actually needs to add an excessive amount of bicarbonate to increase the reaction rate, and at the same time change the temperature multiple times to increase the solubility, and as a result, the product is likely to be mixed with unreacted impurities. The actual purity The situation is not ideal

Method used

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  • A kind of polycyclic carbonate resin and its rapid preparation method and application under normal pressure
  • A kind of polycyclic carbonate resin and its rapid preparation method and application under normal pressure
  • A kind of polycyclic carbonate resin and its rapid preparation method and application under normal pressure

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] (1) Preparation of Hydroxycyclic Carbonate

[0039] The raw material formula of hydroxycyclic carbonate is as table 1:

[0040] Table 1

[0041]

[0042] Preparation method: Add metered glycerin, dimethyl carbonate and potassium carbonate into a three-neck flask equipped with a thermometer, condenser and stirring paddle, raise the temperature to 70°C, keep it warm for 1h, cool down to 40°C and distill under reduced pressure for 1h to remove the by-product methanol and residual dimethyl carbonate, combined with deionized water and potassium carbonate to form hydrated potassium carbonate, to precipitate and remove, after filtering, drop to room temperature and remove water with anhydrous calcium sulfate to obtain hydroxycyclic carbonate.

[0043] Hydroxycyclic carbonate properties: transparent light yellow low viscosity liquid, moisture content < 0.05%, catalyst content < 0.01%, solid content 98%, after drying at 90°C for 2 hours, the hydroxyl value is 478mgKOH / g.

...

Embodiment 2

[0062] 1) Preparation of hydroxycyclic carbonate:

[0063] The formula is shown in Table 5:

[0064] table 5

[0065]

[0066] Preparation method: Add metered glycerin, dimethyl carbonate and potassium hydroxide into a three-neck flask equipped with a thermometer, condenser and stirring paddle, raise the temperature to 60°C, keep it warm for 2.5h, cool down to 40°C, and distill under reduced pressure for 1.2h , remove the by-product methanol and residual dimethyl carbonate, use deionized water to precipitate the catalyst, filter it down to room temperature and dry it with anhydrous calcium sulfate for storage.

[0067] Properties of hydroxycyclic carbonate: transparent light yellow low viscosity liquid, moisture content < 0.05%, catalyst content < 0.05%, solid content 98%, hydroxyl value 474mgKOH / g after drying at 90°C for 2 hours.

[0068] 2). Preparation of cyclocarbonate resin:

[0069] The formula is shown in Table 6:

[0070] Table 6

[0071]

[0072] Preparati...

Embodiment 3

[0083] 1) Preparation of hydroxycyclic carbonate:

[0084] The formula is shown in Table 9:

[0085] Table 9

[0086]

[0087] Preparation method: Add metered glycerin, diethyl carbonate and sodium carbonate into a three-necked flask equipped with a thermometer, condenser and stirring paddle, raise the temperature to 75°C, keep it warm for 0.5h, cool down to 40°C, and distill under reduced pressure for 0.8h. The by-product ethanol and residual diethyl carbonate were removed, the catalyst was precipitated with deionized water, filtered and then cooled to room temperature and stored with anhydrous calcium sulfate.

[0088] Hydroxycyclic carbonate properties: transparent light yellow low viscosity liquid, moisture content < 0.04%, catalyst content < 0.03%, solid content 98%, hydroxyl value 475mgKOH / g after drying at 90°C for 2 hours.

[0089] 2) preparation of cyclocarbonate resin:

[0090] The formula is shown in Table 10:

[0091] Table 10

[0092]

[0093] Preparati...

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Abstract

The invention discloses polycyclic carbonate resin, a normal-pressures rapid preparation method thereof and an application of the resin. The preparation method includes the steps: mixing 11-25wt% of polyhydric alcohols, 75-88wt% of diester carbonate and 0.1-1.0wt% of alkali catalysts, heating mixture to reach the temperature of 60-80 DEG C, and keeping temperature for 0.5-2.5 hours; dissolving isocyanate monomers in solvents, dripping mixture into hydroxy cyclocarbonate, heating mixture to reach the temperature of 40-70 DEG C, keeping the temperature for 0.5-4 hours, and cooling the mixture and discharging the mixture. According to a preparation method of the cyclic carbonate resin, high-temperature and high-pressure conditions are omitted, reaction can be implemented, a reaction system isprovided with a homogeneous phase, an overall process only needs 3-8 hours, conversion rate is high, raw materials are easily acquired, the prepared cyclic carbonate resin is high in purity, a molecular structure is regular, remained -NCO group is omitted, and cyclocarbonate resin solvent type paint synthesized by the cyclic carbonate resin and polyamine has good physical and mechanical properties and chemical resistance and is expected to form green environment-friendly paint replacing traditional polyurethane.

Description

technical field [0001] The present invention relates to a kind of carbonate resin, especially relate to a kind of method of the environment-friendly polycyclic carbonate resin prepared by normal pressure method and the application of resin for preparing non-isocyanate polyurethane coating, the obtained polyurethane coating has good physical and durability Chemical properties. Background technique [0002] Polyurethane (PU) has excellent physical and chemical properties and can be used to make plastics, foams, elastomers, leather, adhesives, sealants, coatings, etc. and used in buildings, electronic products, aircraft, cruise ships, furniture and other fields. In the field of coatings, two-component polyurethane is currently widely used. Two-component polyurethane coatings have excellent properties such as low film-forming temperature, strong adhesion, good abrasion resistance, high hardness, chemical resistance and weather resistance, and are widely used as industrial prot...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G64/30C08G64/12C08G64/02C08G71/04C09D175/04
Inventor 瞿金清戴竟涛吴志军
Owner SOUTH CHINA UNIV OF TECH
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