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Method for producing trifluoro-propyl silicone oil by aid of ion exchange resin

A technology of ion exchange resin and trifluoropropyl silicon, which is applied in the field of producing trifluoropropyl silicone oil with ion exchange resin, can solve the problems of lagging development, difficulty in the synthesis technology of organic fluorine monomers, monopoly, etc., and achieve low production cost , low polymerization reaction temperature, cheap effect

Inactive Publication Date: 2017-12-29
HUBEI XINGRUI SILICON MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] At present, my country's development in the field of new fluorosilicon materials is relatively lagging behind. The main reason is that the synthesis technology of organic fluorine monomers is relatively difficult, and various functional partially fluorine-containing or perfluorinated monomers are still in the experimental synthesis research stage. The production technology of reactive advanced fluoromonomers such as low molecular weight perfluoropolyolefin and perfluoropolyether is basically monopolized by foreign companies

Method used

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  • Method for producing trifluoro-propyl silicone oil by aid of ion exchange resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Take 300g of the by-product of ring distillation and 220g of D3F raw material after pretreatment to a 1000ml three-necked flask (the main components of the by-product of ring distillation are: 22.5% linear siloxane, 64.5% cyclic siloxane, 4.4% Low-boiling organic components, 0.1% trace elements and mechanical impurities.), stir and heat up to 80 ± 5 ℃, dehydration under the conditions of a vacuum of 0.09 MPa for 1 hour, and add a blocking agent (MM quality and water pretreatment after removing the vacuum) After the treatment, the percentage of the sum of the mass of the by-product of the ring distillation and the mass of the raw material D3F, in this example, MM adds 4.5g), heats to 75±5℃, and then adds the catalyst (NHD-6) to the three-necked flask. The addition amount is 5% of the sum of the mass of the by-products of the ring distillation after water pretreatment and the mass of the raw material D3F), react for 1 to 3 hours under normal pressure, stirring speed 200~230...

Embodiment 2

[0024] Take 300g of the by-product of ring distillation and 220g of D3F raw material after pretreatment to a 1000ml three-necked flask (the main components of the by-product of ring distillation are: 20% linear siloxane, 66% cyclic siloxane, 4.3% Low-boiling organic components, 0.05% trace elements and mechanical impurities.), stir and heat up to 80 ± 5 ℃, dehydration under the conditions of a vacuum of 0.09 MPa for 1 h, and add a capping agent (MM quality and water pretreatment after removing the vacuum) After the treatment, the percentage of the sum of the mass of the by-product of the ring body distillation and the mass of the raw material D3F. In this example, MM was added 4.0g), heated to 75±5℃, and then added the catalyst (NHD-6) to the three-necked flask. The addition amount is 5% of the sum of the mass of the by-products of the ring distillation after water pretreatment and the mass of the raw material D3F), react for 1 to 3 hours under normal pressure, stirring speed 20...

Embodiment 3

[0026] Take 300g of the by-product of ring distillation and 220g of D3F raw material after pretreatment to a 1000ml three-necked flask (the main components of the by-product of ring distillation are: 12.5% ​​linear siloxane, 60.9% cyclic siloxane, 3.5% Low-boiling organic components, 0.05% trace elements and mechanical impurities.), stir and heat up to 80 ± 5 ℃, dehydration under the conditions of a vacuum of 0.09 MPa for 1 h, and add a capping agent (MM quality and water pretreatment after removing the vacuum) After the treatment, the percentage of the sum of the mass of the by-product of the ring distillation and the mass of the raw material D3F, in this example, MM adds 4.5g), heats to 75±5℃, and then adds the catalyst (NHD-6) to the three-necked flask. The addition amount is 10% of the sum of the mass of the by-product of ring distillation after water pretreatment and the mass of the raw material D3F), react for 1~3h under normal pressure, stirring speed 200~230r / min, and ho...

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Abstract

The invention discloses a method for producing trifluoro-propyl silicone oil by the aid of ion exchange resin. The method includes pretreating cyclo-rectification byproducts and water to obtain supernatant oil layers, then feeding the supernatant oil layers into a container, feeding 1, 3, 5 (3, 3, 3-trifluoro-propyl) trimethyl cyclo-trisiloxane into the container, uniformly stirring and mixing the supernatant oil layers and the 1, 3, 5 (3, 3, 3-trifluoro-propyl) trimethyl cyclo-trisiloxane with one another to obtain first mixtures, heating the first mixtures, dehydrating the first mixtures under vacuum conditions, adding end-capping agents into the first mixtures after the vacuum is eliminated, adding catalysts into the container to obtain second mixtures, continuing to heat the second mixtures, carrying out reaction under the conditions of the normal pressure and the stirring speed of 200-230 r / min for 1-3 h, then carrying out suction filtration by the aid of filter bags and measuring the conversion rate of filter liquor; pouring filtered liquid materials in three-mouth flasks, then heating the filtered liquid, removing low-boiling-point substances for 1-5 h, placing filtered resin in containers and hermetically storing the filtered resin in the containers. Products are sampled, and indexes of the appearance, the viscosity, the density, volatile matters, the flashing points and the like of the products are detected. The method has the advantages that processes for producing the trifluoro-propyl silicone oil are simple, the trifluoro-propyl silicone oil can be continuously industrially produced by the aid of the method, the products are stable in quality, and index requirements on the indexes of the conversion rate, the viscosity, the density, the volatile matters, the flashing points and the like of the products can be met.

Description

Technical field [0001] The invention belongs to the technical field of chemical organic silicon production, and specifically relates to a method for producing trifluoropropyl silicone oil by using ion exchange resin. Background technique [0002] At present, my country's development in the field of new fluorosilicon materials is relatively lagging. The main reason is that the synthesis of organic fluorine monomers is difficult. Various functional partially fluorinated or perfluorinated monomers are still in the experimental synthesis research stage, with narrow distribution, The production technology of reactive advanced fluoromonomers such as low molecular weight perfluoropolyolefin and perfluoropolyether is basically monopolized by foreign companies. [0003] Fluorosilicone rubber (FVMQ) raw rubber is mainly composed of polymethyltrifluoropropyl silicone (PMFS). PMFS is a high molecular polymer with W-Si-O-Si chain link as the main chain and side groups on the silicon atom being ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/24C08G77/08
CPCC08G77/08C08G77/24
Inventor 尹华金马会娟杜宏伟黄颜锋张红玲
Owner HUBEI XINGRUI SILICON MATERIAL CO LTD
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