CN105254893B - A kind of silicon rubber of low viscosity 107 and preparation method thereof - Google Patents
A kind of silicon rubber of low viscosity 107 and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to adhesive field, and in particular to a kind of silicon rubber of low viscosity 107 and preparation method thereof.Purpose is that providing a kind of course of reaction controls simple, the preparation method of the stable silicon rubber of low viscosity 107 of product viscosity, specifically includes in this method：A, it is dehydrated：Under non-vacuum, dimethyl siloxane mixes ring body under conditions of 80 DEG C~100 DEG C, decompression dehydration 0.5~1.5 hour；B, it is catalyzed：Base catalyst is added when being warming up to 100~115 DEG C, continues to heat up, controlling reaction temperature is at 130~160 DEG C, by balanced reaction time control at 0.5~1.5 hour；C, degrade：Water is added to degrade；D, neutralize：Add nertralizer and carry out neutralization reaction；E, cut is collected：Vacuum is opened after neutralization reaction, and heated material temperature reaches 120~195 DEG C, controls and maintains vacuum 0.08MPa~0.098MPa, cut is collected, untill being oozed without cut.The preparation method high income, the silicon rubber of gained low viscosity 107 can be widely applied in electronics industry and aviation and war industry.
Description
Technical field
The present invention relates to adhesive field, and in particular to a kind of silicon rubber of low viscosity 107 and preparation method thereof.
Background technology
In organosilicon series of products, α, alpha, omega-dihydroxy polydimethyl siloxane (referred to as 107 silicon rubber) is in silicon rubber
One of staple product, such as building, coating, industrial art field suffer from being widely applied in many aspects.Particularly in recent years
Come with the industrialization of Building Trade in China, seriation, high level and superelevation stratification, lighting and full field of view system and large-scale framework extension
A large amount of uses of harden structure, the requirement more and more higher to encapsulant.
Prior art prepare 107 silicon rubber concrete technology be：Dimethyl siloxane mixes ring body (abbreviation DMC) first one
It is dehydrated at fixed temperature and vacuum degree condition, after being warming up to certain temperature, adds base catalyst, ring-opening polymerisation is glued to certain
Degree, rear heating destroy base catalyst, and product then is carried out into de- reduction process.This more difficult control of technique pilot process, was controlled
Unstability be present in journey.
The content of the invention
Present invention aims at providing, a kind of course of reaction control is simple, the stable silicon rubber of low viscosity 107 of product viscosity
Preparation method, be that catalyst is done using alkali in this method, distilled water does end-capping reagent.The viscosity of 107 silicon rubber of the invention is
2000mPas~3000mPas.
Specifically, the preparation method of the silicon rubber of low viscosity 107 of the present invention, comprises the following steps：
A, it is dehydrated：Under non-vacuum, dimethyl siloxane mixes ring body under conditions of 80 DEG C~100 DEG C, decompression
Dehydration 0.5~1.5 hour；
B, it is catalyzed：Add base catalyst when being warming up to 100~115 DEG C, continue to heat up, controlling reaction temperature 130~
160 DEG C, by balanced reaction time control at 0.5~1.5 hour；
C, degrade：Water is added to degrade；
D, neutralize：Add nertralizer and carry out neutralization reaction；
E, cut is collected：Vacuum is opened after neutralization reaction, and heated material temperature reaches 120~195 DEG C (preferably 190
DEG C), control and maintain vacuum collection evaporates for -0.08MPa~-0.098MPa (preferably -0.095MPa~-0.098MPa)
Point, untill being oozed without cut.
In above-mentioned technical proposal, the weight proportion of each material is：Dimethyl siloxane mixes 3500 parts of ring body, base catalysis
0.01~0.07 part of agent, 3.4~17 parts of distilled water, the number of nertralizer is 0.015~0.105 part；
Further preferably, the weight proportion of each material is：Dimethyl siloxane mixes 3500 parts of ring body, base catalyst
0.01~0.07 part, 7 parts of distilled water, nertralizer at least with base catalyst equimolar quality.
In above-mentioned technical proposal, base catalyst includes：Potassium hydroxide, TMAH, tetrabutylammonium hydroxide phosphorus
Or the saline and alkaline glue of silanol, the saline and alkaline glue of the silanol of TMAH, the saline and alkaline glue of the silanol of tetrabutylammonium hydroxide phosphorus of potassium hydroxide
At least one of.
In above-mentioned technical proposal, described nertralizer includes：At least one of carbon dioxide, silicon substrate phosphate, phosphoric acid.
In above-mentioned technical proposal, reaction is carried out in the consersion unit with agitating device and condensing unit.
In above-mentioned technical proposal, balanced reaction time when step B is catalyzed is preferably controlled in 0.5~1h.
In above-mentioned technical proposal, reaction temperature when step B is catalyzed is preferably 140~160 DEG C.
Lead to inert gas (preferably nitrogen) in advance in above-mentioned technical proposal, when step A is dehydrated to enter in consersion unit, and protect
It is to carry out under nitrogen protection to demonstrate,prove whole course of reaction.
In above-mentioned technical proposal, step E collect cut in, take off 120~190 DEG C of low temperature, vacuum be -0.08MPa~-
0.098MPa, preferably vacuum are -0.095MPa~-0.098MPa.Inventor has found through experiment, at 120 DEG C, has small molecule
Therefrom evaporate, with the rise of temperature, small molecule is deviate from more and more, almost all of small when temperature reaches 190 DEG C
Molecule can therefrom be deviate from, therefore it is 120~195 DEG C to select de- low temperature.
The key improvements point of the present invention is that 107 conventional silicon rubber preparation methods are controlled in whole technological processes
Reaction is in vacuum state.But the present invention is in step A dehydrations, step B catalysis, step C degradeds, step D and big
Reacted under the non-vacuum of gas UNICOM, and only evaporating Time-sharing control reaction system in collection is in vacuum state, it is such good
Place is controlled by above-mentioned steps, and 107 silicone rubber products transparencies of preparation are higher, even molecular weight distribution.
By the inventive method prepare 107 silicon rubber viscosity it is relatively low, generally 2000~3000mPas, transparency compared with
Height, molecular weight distribution is more uniform, molecular weight ranges 36000~40000.The silicon rubber of low viscosity 107 in the market is mostly
It is raw material from organosilicon hydrolyzation material, the product transparency of preparation is relatively low, and turbidity scope is 7~9, and molecular weight distribution is wider,
Molecular weight ranges are 18000~58000, it is impossible to be used in the preparation of high transparency silicone adhesive.The present invention be from DMC, preparation
The silicone rubber products transparency of low viscosity 107 is higher, even molecular weight distribution, can be used for the production of high-end silicone adhesive.
The beneficial effects of the invention are as follows：By being effectively controlled to above-mentioned reaction condition, low viscosity 107 can be obtained
Silicone rubber products, the silicone rubber products of low viscosity 107 have in current electronics industry and aviation and war industry and had been widely used
Higher market value, the invention are the silicon rubber of low viscosity 107 using base catalysis composition principle from the raw material DMC that is easy to get
Preparation provides a kind of new control technique and method, and preparation technology is simple, and product viscosity is stable, high income, disclosure satisfy that reality
The needs of border production.
Embodiment
Show the beneficial effect of preparation method of the present invention using screening test below.
3500g dimethyl siloxane mixed methylcyclosiloxanes are added in 5000ml four-hole boiling flask, heating, are stirred simultaneously,
Decompression dehydration 0.5 hour at about 80 DEG C.Continue to heat up, catalyst potassium hydroxide added when temperature is increased to 100~115 DEG C,
Continue to heat up, at 130~160 DEG C, material viscosity gradually increases controlling reaction temperature, will control in the reaction time small 0.5~1.5
When, then to add distilled water and degraded, degraded adds phosphoric acid and carries out neutralization reaction after terminating, neutralization opens vacuum after terminating,
It is heated to temperature of charge and reaches 190 DEG C, vacuum ＞ -0.095MPa, this vacuum is maintained, untill being oozed without cut.
1. influence of the reaction temperature to product
Silicon oxygen bond in ring body will be fragmented into high-molecular compound more than 120 DEG C by strong alkaline substance in theory, and
Also the trend to go up can be presented with the rise of reaction temperature in reaction rate, but too high temperature also results in reaction controlling
Difficulty increase, therefore this experiment use reaction temperature control at 130~160 DEG C, selection 130 DEG C, 135 DEG C, 140 DEG C, 145
DEG C, 150 DEG C, 155 DEG C, 160 DEG C of seven points carry out contrast test, catalyst KOH, dosage 0.05g, polymerization time is
55min, amount of water 7g, degradation time 1h, phosphoric acid addition are 0.058g, and the neutralization time is 40min, is then depressurized
Distillation, deviate from low molecule.Obtained data such as table 1：
Influence of the reaction temperature of table 1 to product
As can be seen from Table 1, the rise of temperature can effectively improve reaction rate, and then improve the viscosity of product, instead
The conversion ratio answered also improves therewith.But in an experiment, if temperature is too high, the viscosity of product will become uncontrolled, stirring
Also become relatively difficult, so 155 DEG C of selection is used as reaction temperature.
2nd, influence of the addition of catalyst to product
The addition of catalyst has considerable influence to product.Very few, the catalytic effect unobvious that catalyst adds, if adding
It is too many, then influence product outward appearance and viscosity.Raw material addition 3500g, dewatering time 30min, catalyst amount 0.01g
~0.07g, polymerization time 55min, amount of water 7g, degradation time 1h, investigate influence of the dosage to product of catalyst.
The catalyst amount of table 2 and the influence of the silicon rubber viscosity of low viscosity 107
From table 2 it can be seen that the viscosity of product increases with the increase of catalyst, but the addition of catalyst is excessive
When, there is considerable influence to the outward appearance of product.Because the product of production must meet Standard, i.e. product need to be water white transparency liquid
Body, therefore the catalyst charge selected is 0.05g.
3rd, influence of the addition of water to product
Polymerisation occurs in the presence of a catalyst for dimethyl siloxane mixed methylcyclosiloxane, when polymerization reaches certain time
Afterwards, water need to be added to degrade to the viscosity of product, the addition of water directly influences the final viscosity of product.7 kinds of selection is not
With addition observe influence of the water to product viscosity, as shown in table 3：
Influence of the addition of the water of table 3 to product
As can be seen from Table 3, the slightly inversely proportional function of the viscosity of the addition of water and 107 silicon rubber, the addition of water are got over
More, the viscosity of 107 silicon rubber is lower.Because a hydrone disconnects a silica silicon key, two hydroxyls are generated.But
Under conditions of degraded, hydroxyl is also very easy to be condensed into water, so this is a dynamic equilibrium, finally can generate that how many hydroxyl take
Certainly in the condition of reaction, when water is more, hydroxyl is easily generated, so to ensure there is enough water in liquid phase as far as possible.But with
The addition of dampening constantly increases, though the once downward trend of the viscosity of product, system occur it is muddy, the turbidity of product also with
Decline.Therefore the addition of the water of this experimental selection is 7g.Sample is made in this experiment 6 and 7, and viscosity is respectively 1700mPas
And 1050mPas, but but some are muddy for product appearance, non-leuco clear viscous liquids, do not meet index request.
4th, influence of the reaction time to product
The scope in reaction time is used as an experimental study point, experiment condition in 30~60min, every 5 minutes：Raw material adds
Enter amount 3500g, dewatering time 30min, catalyst amount 0.05g, amount of water 7g, degradation time 1h, phosphoric acid addition
For 0.058g, the neutralization time is 40min, is then evaporated under reduced pressure, and deviates from low molecule.Obtain result such as table 4：
Influence of the reaction time of table 4 to product viscosity
From table 4, it can be seen that with the extension of time, the viscosity of product can increase therewith, but when viscosity is excessive, production
Degraded after product can go wrong therewith, therefore the polymerization time of selection product is 55min.
The present invention have studied the preparation process of 107 silicon rubber of 2000mPas~3000mPas viscosity, and emphasis is ground
Influence of each reaction condition to product is studied carefully.By investigating each reaction condition and adjustment preparation technology, the 107 of low viscosity is prepared for
Silicon rubber, draw to draw a conclusion：
1) influence of the different reaction temperatures to product viscosity has been investigated by contrast test, it is determined that preferable reaction temperature
It is 155 DEG C.
2) influence of the different reaction time to product viscosity has been investigated by contrast test, it is determined that polymerization reaction time
It is 55min.
3) influence of the different catalyst charges to product viscosity has been investigated by contrast test, it is determined that catalyst
Addition is 0.05g.
4) influence of the addition of different water to product viscosity and turbidity has been investigated by contrast test, it is determined that water
Addition.
5) 2500mPas the and 3000mPas107 silicon rubber index property prepared using this test method is relatively stable,
And client's use is supplied.
Below using the preparating example performance beneficial effects of the present invention of the present invention.
Embodiment 1
By following raw material weight proportioning of soup processed：3500g dimethyl siloxane mixed methylcyclosiloxanes are added to agitating device and condensation
In the vessel of device, heating, while stirring is opened, decompression dehydration 0.5 hour when being warming up to 95 DEG C.Continue to heat up, treat temperature liter
0.05g potassium hydroxide basic catalyst is added at up to 115 DEG C, continues to heat up, controlling reaction temperature is at 155 DEG C, material viscosity
Gradually increase, by balanced reaction time control in 50min, then add 7g distilled water and degraded, degraded adds after terminating etc.
The phosphoric acid of molal weight carries out neutralization reaction, and neutralization slowly opens vacuum after terminating, be heated to temperature of charge reach 190 DEG C, it is true
Reciprocal of duty cycle ＞ -0.095MPa, maintain this vacuum, untill being oozed without cut.Obtaining 2981g (25 DEG C) viscosity is
107 silicone rubber products of 2000mPas water white transparency.Yield is 85%.
Embodiment 2
By following raw material weight proportioning of soup processed：3500g dimethyl siloxane mixed methylcyclosiloxanes are added to agitating device and condensation
In the vessel of device, heating, while stirring is opened, decompression dehydration 0.5 hour when being warming up to 95 DEG C.Continue to heat up, treat temperature liter
0.05g potassium hydroxide basic catalyst is added at up to 115 DEG C, continues to heat up, controlling reaction temperature is at 160 DEG C, material viscosity
Gradually increase, by balanced reaction time control in 55min, then add 7g distilled water and degraded, degraded adds after terminating etc.
The phosphoric acid of molal weight carries out neutralization reaction, and neutralization slowly opens vacuum after terminating, be heated to temperature of charge reach 190 DEG C, it is true
Reciprocal of duty cycle ＞ -0.095MPa, maintain this vacuum, untill being oozed without cut.Obtaining 3086.2g (25 DEG C) viscosity is
107 silicone rubber products of 2600mPas water white transparency.Yield is 88%.
Embodiment 3
By following raw material weight proportioning of soup processed：3500g dimethyl siloxane mixed methylcyclosiloxanes are added to agitating device and condensation
In the vessel of device, heating, while stirring is opened, decompression dehydration 0.5 hour when being warming up to 95 DEG C.Continue to heat up, treat temperature liter
0.05g potassium hydroxide basic catalyst is added at up to 115 DEG C, continues to heat up, controlling reaction temperature is at 155 DEG C, material viscosity
Gradually increase, by balanced reaction time control in 58min, then add 7g distilled water and degraded, degraded adds after terminating
0.075g phosphoric acid carries out neutralization reaction, and neutralization slowly opens vacuum after terminating, is heated to temperature of charge and reaches 175 DEG C, vacuum
＞ -0.095MPa are spent, this vacuum are maintained, untill being oozed without cut.It is 2550mPas to obtain 3325g (25 DEG C) viscosity
Water white transparency 107 silicone rubber products.Yield is 95%.
Embodiment 4
By following raw material weight proportioning of soup processed：3500g dimethyl siloxane mixed methylcyclosiloxanes are added to agitating device and condensation
In the vessel of device, heating, while stirring is opened, decompression dehydration 0.5 hour when being warming up to 95 DEG C.Continue to heat up, treat temperature liter
0.05g potassium hydroxide basic catalyst is added at up to 115 DEG C, continues to heat up, controlling reaction temperature is at 155 DEG C, material viscosity
Gradually increase, by balanced reaction time control in 50min, then add 7g distilled water and degraded, degraded adds after terminating
0.075g phosphoric acid carries out neutralization reaction, and neutralization slowly opens vacuum after terminating, is heated to temperature of charge and reaches 190 DEG C, vacuum
＞ -0.095MPa are spent, this vacuum are maintained, untill being oozed without cut.It is 2500mPas to obtain 3080g (25 DEG C) viscosity
Water white transparency 107 silicone rubber products.Yield is 88%.
Embodiment 5
By following raw material weight proportioning of soup processed：3500g dimethyl siloxane mixed methylcyclosiloxanes are added to agitating device and condensation
In the vessel of device, heating, while stirring is opened, decompression dehydration 0.5 hour when being warming up to 95 DEG C.Continue to heat up, treat temperature liter
0.05g potassium hydroxide basic catalyst is added at up to 115 DEG C, continues to heat up, controlling reaction temperature is at 155 DEG C, material viscosity
Gradually increase, by balanced reaction time control in 60min, then add 7g distilled water and degraded, degraded adds after terminating etc.
The phosphoric acid of molal weight carries out neutralization reaction, and neutralization slowly opens vacuum after terminating, be heated to temperature of charge reach 180 DEG C, it is true
Reciprocal of duty cycle ＞ -0.095MPa, maintain this vacuum, untill being oozed without cut.Obtaining 3290g (25 DEG C) viscosity is
107 silicone rubber products of 2550mPas water white transparency.Yield is 94%.
Embodiment 6
By following raw material weight proportioning of soup processed：3500g dimethyl siloxane mixed methylcyclosiloxanes are added to agitating device and condensation
In the vessel of device, heating, while stirring is opened, decompression dehydration 0.5 hour when being warming up to 95 DEG C.Continue to heat up, treat temperature liter
0.05g potassium hydroxide basic catalyst is added at up to 115 DEG C, continues to heat up, controlling reaction temperature is at 155 DEG C, material viscosity
Gradually increase, by balanced reaction time control in 55min, then add 7g distilled water and degraded, degraded adds after terminating etc.
The phosphoric acid of molal weight carries out neutralization reaction, and neutralization slowly opens vacuum after terminating, be heated to temperature of charge reach 190 DEG C, it is true
Reciprocal of duty cycle ＞ -0.095MPa, maintain this vacuum, untill being oozed without cut.Obtaining 3226.5g (25 DEG C) viscosity is
107 silicone rubber products of 2500mPas water white transparency.Yield is 92%.
Embodiment 1-6 product analysis the results are shown in Table 6：
Table 6：Product analysis result
Note：Professional standard：Turbidity≤3 are Grade As；≤ 7 be certified products.
As seen from the experiment, 107 silicone rubber products that prepared by the present invention, viscosity in 2000~2600mPas, are glued
Spend relatively low, transparency is higher and stable processing technique, reappearance and operability are preferable.
Claims (11)
1. the preparation method of the silicon rubber of low viscosity 107, it is characterized in that：Comprise the following steps：
A, it is dehydrated：Under non-vacuum, dimethyl siloxane mixes ring body under conditions of 80~100 DEG C, decompression dehydration 0.5
~1.5 hours；
B, it is catalyzed：Base catalyst is added when being warming up to 100~115 DEG C, continues to heat up, controlling reaction temperature is 150~160
DEG C, by balanced reaction time control in 50~60min；
C, degrade：Water is added to degrade；
D, neutralize：Add nertralizer and carry out neutralization reaction；
E, cut is collected：Vacuum is opened after neutralization reaction, and heated material temperature reaches 120~195 DEG C, controls and maintains vacuum
Degree -0.08MPa~-0.098MPa, cut is collected, untill being oozed without cut；
Wherein, the weight proportion of each material is：Dimethyl siloxane mixes 3500 parts of ring body, base catalyst 0.04~0.05
Part, 5~7 parts of distilled water, the number of nertralizer is 0.015~0.105 part；
The viscosity of the silicon rubber of low viscosity 107 is 2000mPas~3000mPas.
2. the preparation method of the silicon rubber of low viscosity 107 according to claim 1, it is characterized in that：Step E heated material temperature
Degree reaches 190 DEG C.
3. the preparation method of the silicon rubber of low viscosity 107 according to claim 1, it is characterized in that：Step E maintains vacuum
Degree -0.095MPa~-0.098MPa.
4. the preparation method of the silicon rubber of low viscosity 107 according to claim 1, it is characterized in that：The weight of each material is matched somebody with somebody
Than for：
Dimethyl siloxane mix 3500 parts of ring body, 0.04~0.05 part of base catalyst, 7 parts of distilled water, nertralizer at least with
Base catalyst equimolar quality.
5. the preparation method of the silicon rubber of low viscosity 107 according to Claims 1 to 4 any one, it is characterized in that：It is described
Base catalyst includes：Potassium hydroxide, TMAH, the saline and alkaline glue of the silanol of tetrabutylammonium hydroxide phosphorus or potassium hydroxide,
At least one of the saline and alkaline glue of silanol of TMAH, the saline and alkaline glue of the silanol of tetrabutylammonium hydroxide phosphorus.
6. the preparation method of the silicon rubber of low viscosity 107 according to Claims 1 to 4 any one, it is characterized in that：It is described
Nertralizer include：At least one of carbon dioxide, silicon substrate phosphate, phosphoric acid.
7. the preparation method of the silicon rubber of low viscosity 107 according to claim 1, it is characterized in that：Reaction is with stirring
Mix in the consersion unit of device and condensing unit and carry out.
8. the preparation method of the silicon rubber of low viscosity 107 according to claim 1, it is characterized in that：Step A is advance when being dehydrated
Logical nitrogen enters consersion unit, and whole course of reaction is carried out under inert gas shielding.
9. the preparation method of the silicon rubber of low viscosity 107 according to claim 8, it is characterized in that：The inert gas is
Nitrogen.
10. the preparation method of the silicon rubber of low viscosity 107 according to claim 1, it is characterized in that：Step E collects cut
In, take off 120~190 DEG C of low temperature.
11. the preparation method described in any one of claim 1~10 prepares the silicon rubber of low viscosity 107 of gained.
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| CN105801863B (en) * | 2016-05-10 | 2021-04-02 | 山东大学 | Preparation method of hydroxyl-terminated polymethylethylsiloxane |
| CN106279696A (en) * | 2016-09-27 | 2017-01-04 | 枣阳市华威硅氟材料有限公司 | A kind of production system of 107 silicone rubber |
| CN108912331B (en) * | 2018-07-23 | 2021-08-31 | 湖北兴瑞硅材料有限公司 | Synthesis method of low-viscosity room-temperature vulcanized methyl silicone rubber |
| CN111154106A (en) * | 2019-12-30 | 2020-05-15 | 枣阳市金鹏化工有限公司 | Novel high-viscosity 107 glue and preparation method thereof |
| CN111087620A (en) * | 2019-12-31 | 2020-05-01 | 枣阳市金鹏化工有限公司 | Method for synthesizing 201 methyl silicone oil from waste silicone rubber |
| CN114573813A (en) * | 2022-03-07 | 2022-06-03 | 新疆西部合盛硅业有限公司 | Catalyst and process for preparing 107 glue |
| CN114561014A (en) * | 2022-03-21 | 2022-05-31 | 内蒙古恒星化学有限公司 | Method for synthesizing glue 107 and glue 107 |
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|---|---|---|---|---|
| CN101173044A (en) * | 2007-10-30 | 2008-05-07 | 江苏宏达新材料股份有限公司 | Method for producing 107 adhesive by comprehensive utilization of organosilicon hydrolyzation material loop separation |
| CN102604103A (en) * | 2012-04-11 | 2012-07-25 | 唐山三友硅业有限责任公司 | Preparation method of low volatile matter room temperature vulcanization methyl silicone rubber |
| CN103435807A (en) * | 2013-08-01 | 2013-12-11 | 广东信翼新材料股份有限公司 | Method for preparing odorless and transparent 107 glue at ordinary pressure |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101173044A (en) * | 2007-10-30 | 2008-05-07 | 江苏宏达新材料股份有限公司 | Method for producing 107 adhesive by comprehensive utilization of organosilicon hydrolyzation material loop separation |
| CN102604103A (en) * | 2012-04-11 | 2012-07-25 | 唐山三友硅业有限责任公司 | Preparation method of low volatile matter room temperature vulcanization methyl silicone rubber |
| CN103435807A (en) * | 2013-08-01 | 2013-12-11 | 广东信翼新材料股份有限公司 | Method for preparing odorless and transparent 107 glue at ordinary pressure |
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