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Ultraviolet-curable carboxyl alkyl substituted silicone as well as preparation method and application thereof

A carboxyl silicone oil and ultraviolet light technology, applied in the field of ultraviolet light curing, can solve the problems of carboxyl silicone oil not having photocurable properties, easy to be poisoned, complex synthesis, etc., and achieve the effects of high yield, low odor, and simple preparation method.

Active Publication Date: 2019-07-12
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the traditional synthesis technology is to protect the carboxyl group by esterification first, and then hydrolyze to release the carboxyl group, which is easy to produce by-products, the yield is low, and the synthesis is complicated and costly. The structure of the final product may be different from the pre-designed one.
Prior art CN102731787A discloses a method for preparing carboxyl silicone oil. In this preparation method, dilute acid and chlorosilane are used to directly synthesize carboxyl silicone oil through the direct hydrosilylation reaction, but the catalyst used therein is a platinum catalyst, which is prone to poisoning under acidic conditions. , and the prepared carboxy silicone oil does not have the corresponding light curing performance

Method used

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  • Ultraviolet-curable carboxyl alkyl substituted silicone as well as preparation method and application thereof
  • Ultraviolet-curable carboxyl alkyl substituted silicone as well as preparation method and application thereof
  • Ultraviolet-curable carboxyl alkyl substituted silicone as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0072] A kind of UV curable carboxyl silicone oil, its structural formula is:

[0073]

[0074] Its preparation method is:

[0075] Equipped with stirrer, condenser, nitrogen N 2 In the four-neck bottle of the import and thermometer, add undecylenic acid CH 2 =CH(CH 2 ) 8COOH (49.75g, 0.27mol), n-hexane (224.00g), ethanol (60.00g), Dow Corning DC-4000 (0.30g), oxalic acid (1.50g) and hydrogen-containing polysiloxane 100.00g, at 70°C After reacting for 0.5h, after cooling down to 50-60°C, add methacryloxypropylmethyldiethoxysilane (52.08g, 0.20mol), p-hydroxyanisole (0.48g) and concentrated hydrochloric acid ( 2.02g), under vacuum to -0.095~-0.10MPa, react for 2~3h, add end-capping agent MM (1.01g, 0.0062mol), react for 1h, add glacial ethyl acetate (161.46g) , washed 2 times with ice water, took the oil layer, and distilled under reduced pressure for 40min at a vacuum degree of -0.095~-0.10MPa, 80~85°C to obtain a light yellow transparent viscous substance.

[0076] W...

Embodiment 2

[0082] A kind of ultraviolet curable carboxyl silicone oil, its structural formula is:

[0083]

[0084] Its preparation method is:

[0085] Equipped with stirrer, condenser, nitrogen N 2 In the four-necked bottle of the inlet and the thermometer, add acrylic acid CH 2 = CHCOOH (144.12g, 2.00mol), toluene (346.00g), isopropanol (157.30g), ACS-Pt-40 (0.40g), n-hexanoic acid (4.72g) and hydrogen-containing polysiloxane 170.40g, After reacting at 60°C for 1 hour, after cooling down to 50-60°C, add 3-acryloyloxypropylmethyldimethoxysilane (1091.60g, 5.00mol), polymerization inhibitor 701 (0.38g) and three Fluoromethanesulfonic acid (8.44g), under the vacuum degree reaching -0.095~-0.10MPa, after reacting for 2~3h, add methoxytrimethylsilane TMSOME (10.42g, 0.1mol), after reacting for 3h, add After icing toluene (1687.34g), wash it twice with ice water, take the oil layer, and distill it under reduced pressure for 0.5h at a vacuum degree of -0.095~-0.10MPa, 80~85°C to obtain ...

Embodiment 3

[0092] A kind of ultraviolet curable carboxyl silicone oil, its structural formula is:

[0093]

[0094] Its preparation method is:

[0095] Equipped with stirrer, condenser, nitrogen N 2 In the four-necked bottle of the inlet and the thermometer, add 6-heptenoic acid CH 2 =CH(CH 2 ) 4 COOH (61.52g, 0.48mol), heptane (290.80g), methanol (56.50g), CAT-PL-56 (0.23g), phthalic acid (1.30g) and hydrogenated polysiloxane 100.00g, After reacting at 70°C for 0.5h, after cooling down to 50-60°C, add methacryloyloxymethylmethyldiethoxysilane (46.99g, 0.23mol), hydroquinone (11.12g) and concentrated Sulfuric acid (3.75g), at -0.095~-0.10MPa under vacuum, after reacting for 2~3h, add end-capping agent MD 2 M (4.17g, 0.013mol), after reacting for 2h, add icycyclohexane (375.50g), wash twice with ice water, take the oil layer, under vacuum degree of -0.095~-0.10MPa, 80~85℃, Distilled under reduced pressure for 50min to obtain light yellow transparent sticky matter,

[0096] Where...

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Abstract

The invention discloses ultraviolet-curable carboxyl alkyl substituted silicone as well as a preparation method and an application thereof. The carboxyl alkyl substituted silicone is a modified organic silicon material taking Si-O-Si as a backbone and carboxyl groups and photocuring groups as branches. The ultraviolet-curable carboxyl alkyl substituted silicone contains ultraviolet-curable activegroups, can be rapidly cured under ultraviolet irradiation, is green, energy-saving and environmentally friendly, also has the characteristics of traditional carboxyl alkyl substituted silicone due tointroduction of the carboxyl groups, has thermal stability, corrosion resistance, oxidation stability and the like and is nontoxic, odorless and good in biocompatibility; the existing thermal curingprocess is changed, and the curing process is simple; the silicone oil has excellent storage stability, and storage stability time is about 400 days, the ultraviolet-curable carboxyl alkyl substitutedsilicone with stable performance is prepared with a two-step one-pot method, raw materials are easily available, the preparation method is simple and convenient, reaction conditions are mild, the yield is high, odor is small, and requirements of industrial production are met.

Description

technical field [0001] The invention relates to the field of ultraviolet light curing technology, more specifically, relates to an ultraviolet light curable carboxyl silicone oil and its preparation method and application. Background technique [0002] The polysiloxane with carboxyl group attached to the side chain or the terminal carbon atom is called carboxyl alkyl substituted silicone, which is one of the important functional silicone oils and can be used for fabric surface treatment, leather tanning, functional elastomer materials, medical dressings , packaging materials and other fields. At present, the synthesis methods of carboxyl silicone oil mainly include: (1) introducing carboxyl groups into silane, disiloxane or cyclosiloxane, and then reacting with polysiloxane in equilibrium to prepare carboxypolysiloxane; (2) Condensation of chlorohydrocarbyl siloxane with sodium adipate can obtain carboxyl-terminated polysiloxane, which can be used as a connecting unit of bl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/38
CPCC08G77/38
Inventor 刘珠刘晓暄向洪平李卓尘张晋源
Owner GUANGDONG UNIV OF TECH
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