Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of phenyl hydrogen-containing silicone oil and preparation method thereof

A technology of phenyl hydrogen-containing silicone oil and siloxane, which is applied in the field of organic silicon materials, can solve the problems of poor thermal stability, high price, harsh reaction conditions, etc., so as to avoid the use of neutralizers, avoid harsh use conditions, and improve Yield and Quality Effects

Active Publication Date: 2022-04-19
JIANGSU MAYSTA CHEM
View PDF0 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The moisture-proof and hydrophobic properties of hydrogen-containing silicone oil are better than dimethyl silicone oil, but the thermal stability is poor. The introduction of phenyl group can effectively improve the heat resistance and radioactivity resistance of hydrogen-containing silicone oil
[0003] At present, the catalysts commonly used in the preparation of phenyl silicone oil include strong bases and acidic catalysts, etc., but the use of these catalysts will lead to harsh reaction conditions, complicated preparation processes, some will cause environmental pollution, and some are expensive, resulting in Cost increases, meanwhile, the yield of the prepared phenyl silicone oil is low

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of phenyl hydrogen-containing silicone oil and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0038] In view of this, the application specially proposes a new preparation method of phenyl hydrogen-containing silicone oil, comprising the following steps: reacting the required siloxane raw materials and end-capping agent in the presence of heteropolyacid catalyst conditions for the synthesis reaction to take place.

[0039] Wherein, the heteropolyacid catalyst is obtained by loading phosphomolybdenum heteropolyacid (expressed as PMo) on attapulgite (expressed as AT).

[0040] In this application, the phosphomolybdenum heteropolyacid is composed of NH 4 h 2 PO 4 and (NH 4 ) 6 Mo 7 o 4 4H 2 O is obtained by compounding.

[0041] In an optional embodiment, the molar ratio of phosphorus and molybdenum in the heteropolyacid catalyst can be 1:8-12, such as 1:8, 1:9, 1:10, 1:11 or 1:12, etc., also It can be any other value within the range of 1:8-12.

[0042] In an optional embodiment, the loading (expressed in w) of phosphomolybdenum heteropolyacid in attapulgite can...

Embodiment 1

[0083] (1) Pretreatment of attapulgite

[0084] Add dry unmodified attapulgite to 4.0 mol / L hydrochloric acid solution at a volume ratio of 1:1, stir at 50°C for 6 hours, filter and wash until neutral, and vacuum-dry at 90°C for 12 hours, grind and pass through a 200-mesh sieve to obtain pretreated attapulgite.

[0085] (2) Preparation of phosphomolybdenum heteropoly acid

[0086] Weigh the measured NH according to the molar ratio P:Mo=1.0:10.5 4 h 2 PO 4 and (NH 4 ) 6 Mo 7 o 4 4H 2 O was dissolved in deionized water, nitric acid was added to adjust the pH to 1.0, stirred at 80°C for 6 hours, and dried under vacuum at 110°C for 12 hours.

[0087] (3) Preparation of attapulgite-supported phosphomolybdenum heteropolyacid catalyst

[0088] Dissolve the metered phosphomolybdenum heteropolyacid in absolute ethanol, add the pretreated attapulgite after completely dissolving, ultrasonically treat at 30kHz and stir for 12 hours, and vacuum dry at 110°C for 12 hours to obtain a...

Embodiment 2

[0093] (1) Pretreatment of attapulgite

[0094] Add dry unmodified attapulgite to 3.0mol / L hydrochloric acid solution at a volume ratio of 1:1.5, stir at 50°C for 6 hours under sealed conditions, filter and wash until neutral, and vacuum-dry at 90°C for 12 hours, grind and pass through a 200-mesh sieve to obtain pretreated attapulgite.

[0095] (2) Preparation of phosphomolybdenum heteropoly acid

[0096] Weigh the measured NH according to the molar ratio P:Mo=1.0:12 4 h 2 PO 4 and (NH 4 ) 6 Mo 7 o 4 4H 2 O was dissolved in deionized water, nitric acid was added to adjust the pH to 1.0, stirred at 80°C for 6 hours, and dried under vacuum at 110°C for 12 hours.

[0097] (3) Preparation of attapulgite-supported phosphomolybdenum heteropolyacid catalyst

[0098] Dissolve the metered phosphomolybdenum heteropoly acid in absolute ethanol, add the pretreated attapulgite after completely dissolving, ultrasonically treat at 30kHz and stir for 12 hours, and vacuum dry at 110°...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
viscosityaaaaaaaaaa
viscosityaaaaaaaaaa
viscosityaaaaaaaaaa
Login to View More

Abstract

The invention discloses a phenyl hydrogen-containing silicone oil and a preparation method thereof, belonging to the technical field of organic silicon materials. The preparation method of the phenyl hydrogen-containing silicone oil comprises the following steps: synthesizing the siloxane raw material required for the reaction of the phenyl hydrogen-containing silicone oil and an end-capping agent in the presence of a heteropolyacid catalyst. The heteropolyacid catalyst is obtained by loading phosphomolybdenum heteropolyacid on attapulgite. By using a heteropolyacid catalyst as a catalyst for the synthesis reaction, phenyl hydrogen-containing silicone oil can be synthesized under mild reaction conditions, which is beneficial to energy saving and consumption reduction. At the same time, it can also avoid the use of neutralizing agents, simplify the operation process, and reduce the production In addition, the method can also improve the yield and quality of phenyl hydrogen-containing silicone oil. The phenyl hydrogen-containing silicone oil obtained by the method has higher yield and lower viscosity.

Description

technical field [0001] The invention relates to the technical field of organosilicon materials, in particular to a phenyl hydrogen-containing silicone oil and a preparation method thereof. Background technique [0002] Hydrogen-containing silicone oil is an important silicone product, which is widely used as waterproofing agent, anti-sticking agent and anti-corrosion agent. The moisture-proof and hydrophobic properties of hydrogen-containing silicone oil are better than dimethyl silicone oil, but the thermal stability is poor. The introduction of phenyl group can effectively improve the heat resistance and radiation resistance of hydrogen-containing silicone oil. [0003] At present, the catalysts commonly used in the preparation of phenyl silicone oil include strong bases and acidic catalysts, etc., but the use of these catalysts will lead to harsh reaction conditions, complicated preparation processes, some will cause environmental pollution, and some are expensive, result...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/12C08G77/08
Inventor 何运伟平翔林
Owner JIANGSU MAYSTA CHEM