CN110358027A - A kind of preparation method of self-emulsifying alkylaryl silicone oil - Google Patents
A kind of preparation method of self-emulsifying alkylaryl silicone oil Download PDFInfo
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- CN110358027A CN110358027A CN201810319383.7A CN201810319383A CN110358027A CN 110358027 A CN110358027 A CN 110358027A CN 201810319383 A CN201810319383 A CN 201810319383A CN 110358027 A CN110358027 A CN 110358027A
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- hydrogen content
- silicone oil
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C3/00—Selection of compositions for coating the surfaces of moulds, cores, or patterns
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/12—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes
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- Mechanical Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
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Abstract
The invention discloses a kind of preparation methods of self-emulsifying alkylaryl silicone oil, silicon oil of low hydrogen content is modified jointly using allyl polyether alcohol, styrene and laurylene, silicon oil of low hydrogen content is set on the one hand to obtain the amphiphilic of hydrophilic and oleophilic, there is good compatibility between traditional alkylaryl silicone oil simultaneously, both it can become a kind of demoulding agent emulsion with self-emulsifying, simultaneously can also be used as traditional alkylaryl silicone oil emulsifier come using, relative to conventional composite emulsification system, more excellent stability of emulsion can be improved.
Description
Technical field
The present invention relates to release agent fields, and in particular to a kind of emulsification alkylaryl silicone oil and preparation method thereof.
Background technique
With light-duty low oil consumption passenger car is widelyd popularize, wherein automobile-used aluminium alloy castings include motor body, speed changer
Shell, wheelboss part, bracket class product and labyrinth engine cylinder cover, the lightweight of vehicle body and structural member, which becomes, to become
Gesture, this pushes the innovation and development of aluminium alloy castings manufacture, and as the molding time of aluminium casting is extended considerably, this is to tradition
The more high-temperature resistant of die casting demoulding requires to propose challenge.
Casting mold-releasing agent is a kind of isolated substance between mold and finished product, and metal mold product is prevented to be bonded to mould
Tool, acts a kind of processing aid for being easy to be detached from.Common casting mold-releasing agent can be divided into three classes from product form, water
Base, oil base and powdered mold release agents, wherein water based mold release agent due to good cooling results, pollution-free, cast(ing) surface is bright and clean, be conducive to from
The advantages that dynamicization, is widely used.
Alkylaryl silicone oil is a kind of dimethyl silicone polymer that part methyl is replaced by chain alkyl and phenyl, is had
The characteristics such as low, the strong, high temperature resistant of permeability of surface energy, are a kind of release agent materials haveing excellent performance, are widely used in metal product
Die casting demoulding field, especially aluminium and its alloy die casting demoulding.Relative to other kinds of release agent, alkylaryl silicone oil
There is original advantage during complicated precision part die cast, carbon deposition rate is low, and primary coating can be repeatedly opened, raw
Rear coating performance that is high-efficient, and not influencing product is produced, can be guaranteed between metal product and mold during product molding
Be effectively isolated.Currently, aluminium and its alloy product be widely used in aerospace, automobile manufacture, telecommunications, house ornamentation household electrical appliances,
The fields such as new energy, wherein being required to use alkylaryl silicone oil mold release agent in the forming process of many structural members.
Traditional alkylaryl silicone oil mold release agent be on the basis of silicon oil of low hydrogen content, using styrene, α-methylstyrene,
Si―H addition reaction occurs for the double bond containing monomers such as 1- laurylene, 1-tetradecylene, 1- hexadecylene anti-under the catalysis of platinum catalyst
It should be prepared, wherein the monomer containing phenyl is mainly used for adjusting the heat resistance of release agent, long-chain olefin is mainly used for adjusting
The demolding performace of release agent.But there are some problems for existing silicone oil, and wherein polyether modified silicon oil or OP, NP class emulsifier are compatible
Property is poor, causes alkylaryl silicone oil is unstable after emulsification the phenomenon that floating oil occur.
Self-emulsifying alkylaryl silicone oil provided by the present invention has certain emulsifying capacity under the premise of guaranteeing release property,
Compared to general polyether-modified alkylaryl silicone oil or OP, NP class emulsifier, it has with alkylaryl silicone oil more useful compatible
Property.
Summary of the invention
For solve at present polyether-modified alkylaryl silicone oil or OP, NP class emulsifier its have with alkylaryl silicone oil and more have
The consistency problem of benefit, the present invention provide a kind of self-emulsifying alkylaryl silicone oil and preparation method thereof.
Specifically, the present invention provides a kind of preparation method of self-emulsifying alkylaryl silicone oil, which is characterized in that including following
Step:
(1) 1000g silicon oil of low hydrogen content (hydrogen content 0.8%) and allyl polyethenoxy ether (the Zhejiang Real Madrid of 300-500g are taken
HMX-10) in reaction kettle, it is warming up to 90-110 DEG C, is stirred evenly；
(2) styrene and 475-500g 1- laurylene for taking 440-464g mix and are heated with stirring to 60-70 DEG C.0.25g is added
Karstedt catalyst (wherein platinum content be 2%), heat after 10-20min in being added dropwise in reaction kettle in 30-60min, after
Continue and be warming up to 130 DEG C of unreacted small molecules of vacuum distillations removing after being stirred to react 3h, is cooled to 50 DEG C of dischargings.
Wherein contain following four kinds of structural units in the self-emulsifying alkylaryl silicone molecule structure prepared by the present invention:
、、、
Wherein n, r are integer, n=11.
Relative to existing alkylaryl silicone oil mold release agent, self-emulsifying alkylaryl silicone oil prepared by the present invention has as follows
Feature: (1) being provided simultaneously with release property and emulsifying capacity, is capable of the nanoemulsions of self-emulsifying 100-150nm；It (2) can be as biography
The emulsifier of system alkylaryl silicone oil.Compared to general polyether modified silicon oil or OP, NP class emulsifier, have with alkylaryl silicone oil
There is more useful compatibility, is not in floating oil problem.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiments of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's all other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
Embodiment 1.
Take 1000g silicon oil of low hydrogen content (hydrogen content 0.8%) and allyl polyethenoxy ether (the Zhejiang Real Madrid HMX- of 300g
10) in reaction kettle, 90 DEG C is warming up to, is stirred evenly.
The styrene and 475g 1- laurylene for taking 440g mix and are heated with stirring to 60 DEG C.The Karstedt of 0.25g is added
Catalyst (wherein platinum content be 2%) heats after 10min in being added dropwise in reaction kettle in 30min, continues to rise after being stirred to react 3h
Temperature to 130 DEG C of vacuum distillations remove unreacted small molecule, are cooled to 50 DEG C of dischargings.
Embodiment 2.
Take 1000g silicon oil of low hydrogen content (hydrogen content 0.8%) and allyl polyethenoxy ether (the Zhejiang Real Madrid HMX- of 300g
10) in reaction kettle, 110 DEG C is warming up to, is stirred evenly.
The styrene and 500g 1- laurylene for taking 464g mix and are heated with stirring to 70 DEG C.The Karstedt of 0.25g is added
Catalyst (wherein platinum content be 2%) heats after 15min in being added dropwise in reaction kettle in 50min, continues to rise after being stirred to react 3h
Temperature to 130 DEG C of vacuum distillations remove unreacted small molecule, are cooled to 50 DEG C of dischargings.
Embodiment 3.
Take 1000g silicon oil of low hydrogen content (hydrogen content 0.8%) and allyl polyethenoxy ether (the Zhejiang Real Madrid HMX- of 500g
10) in reaction kettle, 100 DEG C is warming up to, is stirred evenly.
The styrene and 490g 1- laurylene for taking 450g mix and are heated with stirring to 70 DEG C.The Karstedt of 0.25g is added
Catalyst (wherein platinum content be 2%) heats after 20min in being added dropwise in reaction kettle in 60min, continues to rise after being stirred to react 3h
Temperature to 130 DEG C of vacuum distillations remove unreacted small molecule, are cooled to 50 DEG C of dischargings.
Embodiment 4.
Take 1000g silicon oil of low hydrogen content (hydrogen content 0.8%) and allyl polyethenoxy ether (the Zhejiang Real Madrid HMX- of 450g
10) in reaction kettle, 110 DEG C is warming up to, is stirred evenly.
The styrene and 500g 1- laurylene for taking 464g mix and are heated with stirring to 65 DEG C.The Karstedt of 0.25g is added
Catalyst (wherein platinum content be 2%) heats after 10min in being added dropwise in reaction kettle in 30min, continues to rise after being stirred to react 3h
Temperature to 130 DEG C of vacuum distillations remove unreacted small molecule, are cooled to 50 DEG C of dischargings.
Claims (9)
1. a kind of preparation method of self-emulsifying alkylaryl silicone oil, it is characterised in that synthetic method is as follows:
(1) 1000g silicon oil of low hydrogen content (hydrogen content 0.8%) and allyl polyethenoxy ether (the Zhejiang Real Madrid of 300-500g are taken
HMX-10) in reaction kettle, it is warming up to 90-110 DEG C, is stirred evenly；
(2) it takes the styrene of 440-464g and 475-500g 1- laurylene to mix and is heated with stirring to 60-70 DEG C, addition 0.25g
Karstedt catalyst (wherein platinum content be 2%), heat after 10-20min in being added dropwise in reaction kettle in 30-60min, after
Continue and be warming up to 130 DEG C of unreacted small molecules of vacuum distillations removing after being stirred to react 3h, is cooled to 50 DEG C of dischargings.
2. preparation method according to claim 1, it is characterised in that the molecule of prepared self-emulsifying alkylaryl silicone oil
There are following four kinds of structural units in structure:
、、、
Wherein n, r are integer, n=11.
3. preparation method according to claim 1, it is characterised in that the hydrogen content of used silicon oil of low hydrogen content is 0.8%.
4. preparation method according to claim 1, it is characterised in that the matter of silicon oil of low hydrogen content and allyl polyethenoxy ether
Amount is than being 1000:300-500.
5. allyl polyethenoxy ether according to claim 4, it is characterised in that hydroxyl value 113mgKOH/g, iodine number are
48gI2/g。
6. preparation method according to claim 1, it is characterised in that the mass ratio of styrene and laurylene is 440-464:
475-500。
7. two kinds of alkene according to claim 6, it is characterised in that Karstedt is first added under conditions of 60-70 DEG C and urges
Agent is stirred to react 10 ~ 20min.
8. the mixed olefins after catalyst reaction are added according to claim 7, it is characterised in that by it in 30 ~ 60min
It is added drop-wise in reaction kettle and silicon oil of low hydrogen content is reacted.
9. preparation method according to claim 1, it is characterised in that the temperature of the stage of reaction is controlled at 90-110 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810319383.7A CN110358027A (en) | 2018-04-11 | 2018-04-11 | A kind of preparation method of self-emulsifying alkylaryl silicone oil |
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| CN201810319383.7A CN110358027A (en) | 2018-04-11 | 2018-04-11 | A kind of preparation method of self-emulsifying alkylaryl silicone oil |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101402734A (en) * | 2008-11-11 | 2009-04-08 | 宁波润禾化学工业有限公司 | Process for producing long-chain alkyl-phenyl modified silicone oil |
| CN105218826A (en) * | 2015-08-28 | 2016-01-06 | 苏州兴业材料科技股份有限公司 | A kind of modified silicon oil and water base casting mold-releasing agent therefrom |
| CN105367802A (en) * | 2015-11-20 | 2016-03-02 | 陕西科技大学 | Polyether modified phenyl hydrogen-containing silicone oil and preparation method thereof |
| CN106084235A (en) * | 2016-06-21 | 2016-11-09 | 南雄鼎成新材料科技有限公司 | A kind of silicon wax emulsifying agent |
| CN107614150A (en) * | 2015-06-26 | 2018-01-19 | 尤希路化学工业有限公司 | Releasing agent used for casting composition |
-
2018
- 2018-04-11 CN CN201810319383.7A patent/CN110358027A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101402734A (en) * | 2008-11-11 | 2009-04-08 | 宁波润禾化学工业有限公司 | Process for producing long-chain alkyl-phenyl modified silicone oil |
| CN107614150A (en) * | 2015-06-26 | 2018-01-19 | 尤希路化学工业有限公司 | Releasing agent used for casting composition |
| CN105218826A (en) * | 2015-08-28 | 2016-01-06 | 苏州兴业材料科技股份有限公司 | A kind of modified silicon oil and water base casting mold-releasing agent therefrom |
| CN105367802A (en) * | 2015-11-20 | 2016-03-02 | 陕西科技大学 | Polyether modified phenyl hydrogen-containing silicone oil and preparation method thereof |
| CN106084235A (en) * | 2016-06-21 | 2016-11-09 | 南雄鼎成新材料科技有限公司 | A kind of silicon wax emulsifying agent |
Non-Patent Citations (1)
| Title |
|---|
| 韩闪闪等: ""烯丙醇聚醚改性硅油的合成"", 《天津工业大学学报》 * |
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Application publication date: 20191022 |