CN106832298A - A kind of resin catalyst is used for the synthetic method of silicon oil of low hydrogen content - Google Patents
A kind of resin catalyst is used for the synthetic method of silicon oil of low hydrogen content Download PDFInfo
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- CN106832298A CN106832298A CN201710089363.0A CN201710089363A CN106832298A CN 106832298 A CN106832298 A CN 106832298A CN 201710089363 A CN201710089363 A CN 201710089363A CN 106832298 A CN106832298 A CN 106832298A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
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Abstract
A kind of resin catalyst is used for the synthetic method of silicon oil of low hydrogen content, and it is raw material with containing hydrogen silicone oil high to use octamethylcy-clotetrasiloxane, and HMDO is end-capping reagent, under the catalysis of resin catalyst, stirs and heats；Filtering purification, decompression is de- low, obtains silicon oil of low hydrogen content.The preparation method of the silicon oil of low hydrogen content is as follows：A certain amount of octamethylcy-clotetrasiloxane, containing hydrogen silicone oil high, HMDO and resin catalyst are weighed in the four-hole boiling flask with agitating device, is stirred and is heated, 3.0 7.5h are reacted at 75 DEG C of temperature 40 DEG C of control；Filtering, filters catalyst purification, after to carry out decompression de- low, remove low molecule；Obtain the neutral silicon oil of low hydrogen content of water white transparency.The present invention uses resin catalyst, in the case where catalytic effect is not influenceed, it is not necessary to neutralizes washing, is easily separated, reusable, and the time is short used by whole preparation process.Product without tart flavour, in neutral transparent.
Description
Technical field
The present invention relates to the synthetic method that a kind of resin catalyst is used for silicon oil of low hydrogen content, belong to chemical technology field.
Background technology
Silicone oil has excellent heat-resisting, weather-proof, insulating properties and physiological inertia, particularly containing hydrogen silicone oil and vinyl silicone oil
With reactive group, synthesis modification siloxanes is often used to.
The conventional method for preparing silicon oil of low hydrogen content often makees catalyst with the concentrated sulfuric acid.The method cannot meet production requirement, general
Store-through is the shortcomings of quality, active not high and big smell.The concentrated sulfuric acid has strong oxidizing property, can etching apparatus；It needs to use after reaction
Sodium acid carbonate is neutralized, washing, increases cost, pollutes environment；Product carries tart flavour, influences it to use scope.
The content of the invention
The purpose of the present invention is that the problem that the catalyst for preparing silicon oil of low hydrogen content for tradition is present, the present invention provides one
Planting resin catalyst is used for the synthetic method of silicon oil of low hydrogen content, and used catalyst is easily separated, reusable, reduces cost；Institute
The no acidic smell of product, in neutral transparent.
The technical scheme is that：
A kind of resin catalyst of the present invention is used for the synthetic method of silicon oil of low hydrogen content, and methods described uses the silicon of prestox ring four
Oxygen alkane D4It is raw material with 202 containing hydrogen silicone oils high, HMDO MM is end-capping reagent, under the catalysis of resin catalyst, is stirred
Mix and heat.Filtering purification, decompression is de- low, obtains silicon oil of low hydrogen content.
The preparation method of catalyst of the present invention is as follows：
A certain amount of octamethylcy-clotetrasiloxane, containing hydrogen silicone oil high, HMDO and resin catalyst are weighed in band
Have in the four-hole boiling flask of agitating device, stir and heat, 3.0-7.5h is reacted at 40 DEG C -75 DEG C of temperature of control.Filtering, filters and urges
Agent is purified, after to carry out decompression de- low, remove low molecule.Obtain the neutral silicon oil of low hydrogen content of water white transparency.
The resin catalyst is D006 type isobutenes catalyst for etherification, D006-2 type isobutenes catalyst for etherification, KC101
Type acid esterification catalyst, KC102 type alkylation of phenol catalyst, KC103 type nonyl phenols alkylation catalyst, DHC-1 types third
Certain in alkene hydration catalyst is several, and its consumption is the 1%-7% of raw material；
The octamethylcy-clotetrasiloxane is (3~3.5) with the mass ratio of containing hydrogen silicone oil high: 1.
Described end-capping reagent consumption is the 1.0%-2.4% of raw material, can be specific to formulate by regulating and controlling end-capping reagent MM consumptions
The silicon oil of low hydrogen content of viscosity.
Preferably, a kind of above-mentioned resin catalyst is used for the synthesis of silicon oil of low hydrogen content, described product is low hydrogeneous
The range of viscosities of silicone oil can be controlled in 40-140mm2/s。
Preferably, a kind of above-mentioned resin catalyst is used for the synthesis of silicon oil of low hydrogen content, described product is low hydrogeneous
The yield of silicone oil can reach more than 90%.
In containing hydrogen silicone oil preparation, end-capping reagent MM has a great impact to containing hydrogen silicone oil properties of product.Its consumption is bigger, produces
Thing chain length is shorter, and viscosity is also smaller, mobility enhancing.Therefore, the silicon oil of low hydrogen content of particular viscosity is formulated, can be adjusted according to following table
Control the consumption of end-capping reagent.End-capping reagent consumption is as shown in the table to the influence reacted.
| Sequence number | MM consumptions (%) | Viscosity (mPa.s) | The amount containing H (%) |
| 1 | 1.0 | 124 | 0.378 |
| 2 | 1.2 | 113 | 0.374 |
| 3 | 1.4 | 99 | 0.371 |
| 4 | 1.6 | 87 | 0.369 |
| 5 | 1.8 | 75 | 0.367 |
| 6 | 2.0 | 65 | 0.364 |
| 7 | 2.2 | 54 | 0.361 |
| 8 | 2.4 | 46 | 0.359 |
Present invention has the advantages that：The present invention uses resin catalyst, in the case where catalytic effect is not influenceed, it is not necessary to neutralize water
Wash, easily separated, it is reusable, and the time is short used by whole preparation process.Product without tart flavour, in neutral transparent.
Brief description of the drawings
Fig. 1 is the reacting flow chart that resin catalyst of the present invention prepares silicon oil of low hydrogen content；
Fig. 2 is the infrared spectrogram of product；
Fig. 3 is the nuclear magnetic resonance H spectrograms of product.
Specific embodiment
Specific embodiment of the invention is as shown in Figure 1.Fig. 1 is that resin catalyst of the present invention prepares the anti-of silicon oil of low hydrogen content
Answer flow chart.
Embodiment 1：
It is 3.19 to weigh mass ratio:1 D4With 202 containing hydrogen silicone oils high, the resin catalyst of 1%MM and 6% is in stirring
Mix in the four-hole boiling flask of device, stir and heat, 6h is reacted under control temperature 60 C.Filtering, filter catalyst purification, after carry out
Decompression is de- low, removes low molecule.Obtain the neutral silicon oil of low hydrogen content of water white transparency.
The viscosity of the silicon oil of low hydrogen content as obtained by the present embodiment is 124mPas.
Embodiment 2
It is 3.25 to weigh mass ratio:1 D4With 202 containing hydrogen silicone oils high, 1.4%MM and 6% resin catalyst in stirring
Mix in the four-hole boiling flask of device, stir and heat, 6h is reacted under control temperature 60 C.Filtering, filter catalyst purification, after carry out
Decompression is de- low, removes low molecule.Obtain the neutral silicon oil of low hydrogen content of water white transparency.
The viscosity of the silicon oil of low hydrogen content as obtained by the present embodiment is 99mPas.
Embodiment 3
It is 3.31 to weigh mass ratio:1 D4With 202 containing hydrogen silicone oils high, 2%MM and 6% resin catalyst in stirring
In the four-hole boiling flask of device, stir and heat, 6h is reacted under control temperature 60 C.Filtering, filter catalyst purification, after subtracted
Pressure-off is low, removes low molecule.Obtain the neutral silicon oil of low hydrogen content of water white transparency.
The viscosity of the silicon oil of low hydrogen content as obtained by the present embodiment is 65mPas.
Embodiment 4
It is 3.35 to weigh mass ratio:1 D4With 202 containing hydrogen silicone oils high, 2.4%MM and 6% resin catalyst in stirring
Mix in the four-hole boiling flask of device, stir and heat, 6h is reacted under control temperature 60 C.Filtering, filter catalyst purification, after carry out
Decompression is de- low, removes low molecule.Obtain the neutral silicon oil of low hydrogen content of water white transparency.
The viscosity of the silicon oil of low hydrogen content as obtained by the present embodiment is 46mPas.
Fig. 2 is the infrared spectrogram of product.By infrared spectrum analysis, in 2950cm-1The absworption peak for nearby occurring is C-H
The stretching vibration peak of key；In 2160cm-1、917cm-1Nearby there is obvious absworption peak, there is Si -- H bond to deposit in this explanation product
；In 1060cm-1Nearby there is obviously absworption peak, there is Si-O keys in this explanation product.These characteristic absorption peaks
Presence characterize the basic structure that containing hydrogen silicone oil has, it was demonstrated that product is strictly containing hydrogen silicone oil, with design structure one
Cause.
Fig. 3 is the nuclear magnetic resonance H spectrograms of product.δ=4.7-4.9 is the proton peak of Si-H in figure, is Si- at δ=0-0.5
CH3In-CH3Hydrogen Proton peak, at δ=7.3 be CDCl3Solvent peak.The product for illustrating synthesis is containing hydrogen silicone oil.
Claims (5)
1. a kind of resin catalyst is used for the synthetic method of silicon oil of low hydrogen content, it is characterised in that methods described uses prestox ring
Tetrasiloxane is raw material with containing hydrogen silicone oil high, and HMDO is end-capping reagent, and under the catalysis of resin catalyst, stirring is simultaneously
Heating；Filtering purification, decompression is de- low, obtains silicon oil of low hydrogen content；
The preparation method of the silicon oil of low hydrogen content is as follows：
A certain amount of octamethylcy-clotetrasiloxane, containing hydrogen silicone oil high, HMDO and resin catalyst are weighed in stirring
Mix in the four-hole boiling flask of device, stir and heat, 3.0-7.5h is reacted at 40 DEG C -75 DEG C of temperature of control；Filtering, filters catalyst
Purification, after to carry out decompression de- low, remove low molecule；Obtain the neutral silicon oil of low hydrogen content of water white transparency.
2. a kind of resin catalyst according to claim 1 is used for the synthetic method of silicon oil of low hydrogen content, it is characterised in that institute
Resin catalyst is stated for D006 type isobutenes catalyst for etherification, D006-2 type isobutenes catalyst for etherification, KC101 type acid esterifications
Catalyst, KC102 type alkylation of phenol catalyst, KC103 type nonyl phenols alkylation catalyst, the catalysis of DHC-1 types propylene hydration
At least one in agent, its consumption is the 1%-7% of raw material.
3. a kind of resin catalyst according to claim 1 is used for the synthetic method of silicon oil of low hydrogen content, it is characterised in that institute
The 1.0%-2.4% that end-capping reagent consumption is raw material is stated, the low Silicon Containing Hydrogen of particular viscosity can be formulated by regulating and controlling end-capping reagent MM consumptions
Oil.
4. a kind of resin catalyst according to claim 1 is used for the synthetic method of silicon oil of low hydrogen content, it is characterised in that institute
State octamethylcy-clotetrasiloxane is with the mass ratio of containing hydrogen silicone oil high（3~3.5）:1.
5. a kind of resin catalyst according to claim 1 is used for the synthetic method of silicon oil of low hydrogen content, it is characterised in that institute
The range of viscosities for stating neutral silicon oil of low hydrogen content is 40-140mm2/s。
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| Application Number | Priority Date | Filing Date | Title |
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| CN2017100138354 | 2017-01-10 | ||
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103524743A (en) * | 2013-07-01 | 2014-01-22 | 江苏天辰硅材料有限公司 | Preparation method of hydrogen-containing silicone oil with terminal hydrogen group |
| CN103665380A (en) * | 2013-12-27 | 2014-03-26 | 蓝星化工新材料股份有限公司江西星火有机硅厂 | Preparation method for low hydrogen-containing silicon oil |
| CN105384934A (en) * | 2015-09-21 | 2016-03-09 | 江西蓝星星火有机硅有限公司 | Preparation method of terminal hydrogen-containing silicone oil |
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- 2017-02-20 CN CN201710089363.0A patent/CN106832298A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103524743A (en) * | 2013-07-01 | 2014-01-22 | 江苏天辰硅材料有限公司 | Preparation method of hydrogen-containing silicone oil with terminal hydrogen group |
| CN103665380A (en) * | 2013-12-27 | 2014-03-26 | 蓝星化工新材料股份有限公司江西星火有机硅厂 | Preparation method for low hydrogen-containing silicon oil |
| CN105384934A (en) * | 2015-09-21 | 2016-03-09 | 江西蓝星星火有机硅有限公司 | Preparation method of terminal hydrogen-containing silicone oil |
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