CN109762011A - A kind of preparation method of functionality amino silane oligomer - Google Patents
A kind of preparation method of functionality amino silane oligomer Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of functional amino silane oligomer, belong to technical field of fine.The present invention is hydrolyzed reaction, chloropropyl alkoxy silane hydrolysate through chloropropyl alkoxy silane and is hydrolyzed after reacting with amino silane progress aminating reaction, amino silane, dechlorination reaction is carried out by using sodium alkoxide, distillation, the filter progress etc. for carrying out low boiling after the reaction was completed obtain the functional amino silane oligomer product of light-coloured transparent, low viscosity, low free chlorine, products of the present invention molar yield reaches 99.0% or more, it can effectively solve the problems, such as existing aminosilane polymer product xanthochromia, be suitble to industrial-scale production；It is particularly suitable for improving the polymer such as room temperature vulcanized silicone rubber, two component polyurethane, organic silicon modified polyurethane, organosilicon modified polyether, bi-component epoxide-resin and inorganic surfaces, the cementability of frosting and wellability.
Description
Technical field
The present invention relates to a kind of preparation methods of functional amino silane oligomer, belong to technical field of fine.
Background technique
Silane low polymer since the advent of the world, just with its unique organic and inorganic structure, excellent resistant of high or low temperature, weather-proof
The performances such as property, dielectricity, low surface tension, physiological inertia, easy to process be widely used in electronics, electric appliance, traffic, aerospace, building,
The fields such as weaving, papermaking, leather, food, medicine, health are a kind of rising novel " green materials ".Currently,
There are many commercially available aminosilane polymer product, but 90% or more is amine ethyl Asia aminopropylpolysiloxane, has 2 on strand
A active hydrogen atom, therefore, the downstream product synthesized using commercially available aminosilane polymer product are equal to a certain extent
Defect with xanthochromia, while having certain deficiency in terms of volatility, ageing-resistant performance and environmental pollution, therefore, have
Necessity makes improvements.
Summary of the invention
It is an object of the invention to: provide it is a kind of can effective solution aminosilane polymer xanthochromia problem, and can
Realize industrialized production, and volatility is low, ageing-resistant performance is good, environmental pollution is small, the functionality with lower VOC emission
The preparation method of amino silane oligomer.
The technical scheme is that
A kind of preparation method of functionality amino silane oligomer, it is characterised in that: it the following steps are included:
1) chloropropyl alkoxy silane product, is added in the three-necked flask A for being connected with reflux condenser (logical down cycles water),
The mixed liquor that deionized water, solvent and hydrochloric acid are added in the constant pressure funnel A of three-necked flask A is connected, wherein chloropropyl alcoxyl
Base silane and the molar ratio of deionized water are 0.75, and the mass ratio of solvent and deionized water is 1:2.0, and hydrochloric acid additional amount is
The 0.03% of chloropropyl alkoxy silane inventory；
2) after, stocking up, magnetic stirring apparatus is opened, oil bath heating device is opened, after temperature of charge reaches 70 DEG C, by constant pressure
The mixing of dropping funel A slowly, in uniform instillation three-necked flask A carries out the hydrolysis of chloropropyl alkoxy silane, hydrolysis
It is 70 ~ 80 DEG C that reaction temperature is controlled in reaction process；Mixing time for adding is 2-4h；
3) after, mixing is added dropwise, under the conditions of control reaction temperature is 80 ~ 90 DEG C, aging reaction 2h is carried out, to ensure deionization
Water fully reacting, after, chloropropyl alkoxy silane hydrolysate is down to room temperature；
4) amino silane product, is thrown in the three-necked flask B for being connected with reflux condenser (logical down cycles water), in three mouthfuls of burnings of connection
Chloropropyl alkoxy silane hydrolysate is put into the constant pressure funnel B of bottle B, wherein amino silane and chloropropyl alkoxy silane
Molar ratio be 1:0.1 ~ 0.3；
5) after feeding intake, magnetic stirring apparatus is opened, oil bath heating device is opened, after temperature of charge reaches 70 DEG C, by constant pressure addition
Chloropropyl alkoxy silane hydrolysate in funnel B slowly, in uniform instillation three-necked flask B carries out chloropropyl alkoxy silane
With the aminating reaction of amino silane, the H atom of amino silane is reacted away, it is 70 that reaction temperature is controlled during aminating reaction
~80℃；
6) after hydrolysate is added dropwise, under the conditions of control reaction temperature is 80 ~ 90 DEG C, aging reaction 2h is carried out, to ensure amination
Fully reacting, after, the temperature of charge in three-necked flask B is reduced to 70 ~ 80 DEG C；
7) deionized water and solvent mixed liquor are thrown in constant pressure funnel B, wherein the mass ratio of deionized water and solvent is
The molar ratio of 1:1, deionized water and amino silane is 0.75；
8) after stocking up, the deionized water mixed liquor in constant pressure funnel B slowly, is uniformly instilled in three-necked flask B
The hydrolysis for carrying out amino silane, control reaction temperature is 70 ~ 80 DEG C in hydrolysis reaction, and the instillation time of mixed liquor is
2—4h；
9) after mixed liquor is added dropwise, control reaction temperature be 80 ~ 90 DEG C under the conditions of, carry out aging reaction 2h, with ensure from
Sub- water fully reacting, after, the temperature of charge in three-necked flask B is reduced to 50 ~ 60 DEG C；
10) after aging reaction, suitable alcohol sodium solution is put into constant pressure funnel B, is then slowly dropped into three mouthfuls of burnings
It carries out neutralizing dechlorination reaction in bottle B, controls 50-60 DEG C of temperature during neutralization reaction；
11) after alcohol sodium solution is added dropwise, heat temperature raising gradually is carried out to three-necked flask B, the solvent in three-necked flask B is steamed
Out, after solvent distillation, the material in three-necked flask B is reduced to room temperature, is then filtered, light, low viscosity, low is obtained
The functional amino silane oligomer product of free chlorine.
The solvent is methanol or ethyl alcohol.
The chloropropyl alkoxy silane product be r-chloropropyl trimethoxyl silane or chloropropyl triethoxysilane,
Or chloropropylmethyldimethoxysilane.
The amino silane is 3- aminopropyl trimethoxysilane or 3- aminopropyl triethoxysilane or N-(2- ammonia
Ethyl) -3- aminopropyl trimethoxysilane product.
The invention has the benefit that
The preparation method of the functionality amino silane oligomer it is raw materials used for amino silane, chloropropyl alkoxy silane, go from
Sub- water, since amino silane is stronger than the hydrolysing activity of chloropropyl alkoxy silane, the present invention is carried out through chloropropyl alkoxy silane
Hydrolysis, chloropropyl alkoxy silane hydrolysate carry out aminating reaction with amino silane, amino silane is hydrolyzed after reacting,
Dechlorination reaction is carried out by using sodium alkoxide, distillation, the filter progress etc. for carrying out low boiling after the reaction was completed obtain light-coloured transparent, low viscous
The functional amino silane oligomer product of degree, low free chlorine, products of the present invention molar yield reach 99.0% or more,
It can effectively solve the problems, such as existing aminosilane polymer product xanthochromia, be suitble to industrial-scale production；The product of synthesis and city
The amino silane oligomer sold, which is compared, has strong lower VOC emission, bonding force, polyfunctionality, low-yellowing, splendid water resistance etc.
Advantage can be widely used for the field of coating, adhesive, sealant, plastics, powder and metal, while because of chloropropyl alkoxyl silicone
The insertion of alkane, to material interface wellability with super strength, can be formed with adhesive substance surface has the product that the present invention synthesizes
Strong weatherability and strong moisture-proof, while there is excellent hydrophobicity, it is particularly suitable for improving room temperature vulcanized silicone rubber, bi-component polyurethane
The polymer such as ester, organic silicon modified polyurethane, organosilicon modified polyether, bi-component epoxide-resin and inorganic surfaces, frosting
Cementability and wellability.
Specific embodiment
Embodiment 1
198g r-chloropropyl trimethoxyl silane is added in the three-necked flask A for being connected with reflux condenser (logical down cycles water) to produce
Product put into 13.5g deionized water, 27g methanol and 0.06g mixed in hydrochloric acid in the constant pressure funnel A of connection three-necked flask A
Expect, after stock, opens magnetic stirring apparatus, oil bath heating device is opened, after temperature of charge reaches 70 DEG C, by constant pressure addition
The mixing of funnel A slowly, in uniform instillation three-necked flask A carries out the hydrolysis of r-chloropropyl trimethoxyl silane, and hydrolysis is anti-
It should control reaction temperature be in the process 70 ~ 80 DEG C, after mixing is added dropwise, under the conditions of control reaction temperature is 80 ~ 90 DEG C, progress
Aging reaction 2h, to ensure deionized water fully reacting, after, r-chloropropyl trimethoxyl silane hydrolysate is down to room temperature.
895g3- aminopropyl trimethoxysilane is thrown in the three-necked flask B for being connected with reflux condenser (logical down cycles water)
Product puts into r-chloropropyl trimethoxyl silane hydrolysate in the constant pressure funnel B of connection three-necked flask B, after stock,
Magnetic stirring apparatus is opened, oil bath heating device is opened, after temperature of charge reaches 70 DEG C, by the chlorine third in constant pressure funnel B
Base trimethoxy silane hydrolysate slowly, in uniform instillation three-necked flask B carries out r-chloropropyl trimethoxyl silane and 3- ammonia third
The aminating reaction of base trimethoxy silane, the H atom of amino silane is reacted away, and reaction temperature is controlled during aminating reaction
It is 70 ~ 80 DEG C, after hydrolysate is added dropwise, under the conditions of control reaction temperature is 80 ~ 90 DEG C, aging reaction 2h is carried out, to ensure
Aminating reaction is complete, and after aminating reaction, the temperature of charge in three-necked flask B is reduced to 70 ~ 80 DEG C, then drips in constant pressure
Throw 67.5g deionized water and 67.5g methyl alcohol mixed liquor in liquid funnel B, after stock, by constant pressure funnel B go from
Sub- water and methyl alcohol mixed liquor slowly, in uniform instillation three-necked flask B carry out the hydrolysis of 3- aminopropyl trimethoxysilane,
It is 70 ~ 80 DEG C that reaction temperature is controlled in hydrolysis reaction, after deionized water and methyl alcohol mixed liquor are added dropwise, control reaction temperature
Under the conditions of degree is 80 ~ 90 DEG C, aging reaction 2h is carried out, it is ensured that deionized water fully reacting, after, it will be in three-necked flask B
Temperature of charge is reduced to 50 ~ 60 DEG C, 195g sodium methoxide solution is then thrown in constant pressure funnel B, and be slowly dropped into three mouthfuls of burnings
It carries out neutralizing dechlorination reaction in bottle B, controls 50-60 DEG C of kettle temperature during neutralization reaction, after sodium methoxide solution is added dropwise, gradually
Heat temperature raising is carried out to three-necked flask B, the methanol in three-necked flask B is steamed, after methanol distills, by three-necked flask B
Interior material is reduced to room temperature, is then filtered to obtain light-coloured transparent, low viscosity, the functional amino silane of low free chlorine low
Copolymer product.
Embodiment 2
240g throws chloropropyl triethoxysilane product in the three-necked flask A for being connected with reflux condenser (logical down cycles water),
13.5g deionized water, 27g ethyl alcohol and 0.07g mixed in hydrochloric acid material are put into the constant pressure funnel A of connection three-necked flask A, it is standby
After material, magnetic stirring apparatus is opened, oil bath heating device is opened, after temperature of charge reaches 70 DEG C, by constant pressure funnel A
Interior mixing slowly, in uniform instillation three-necked flask A carries out the hydrolysis of chloropropyl triethoxysilane, hydrolysis mistake
It is 70 ~ 80 DEG C, after mixing is added dropwise that reaction temperature is controlled in journey, under the conditions of control reaction temperature is 80 ~ 90 DEG C, carries out aging
2h is reacted, to ensure deionized water fully reacting, after, chloropropyl triethoxysilane hydrolysate is down to room temperature.
1105g3- aminopropyl-triethoxy silicon is thrown in the three-necked flask B for being connected with reflux condenser (logical down cycles water)
Alkane product throws chloropropyl triethoxysilane hydrolysate in the constant pressure funnel B on connection three-necked flask B, and stock finishes
Afterwards, magnetic stirring apparatus is opened, oil bath heating device is opened, after temperature of charge reaches 70 DEG C, by the chlorine in constant pressure funnel B
Propyl-triethoxysilicane hydrolysate slowly, in uniform instillation three-necked flask B carries out chloropropyl triethoxysilane and 3- ammonia
The aminating reaction of propyl-triethoxysilicane, the H atom of amino silane is reacted away, and reaction temperature is controlled during aminating reaction
Degree is 70 ~ 80 DEG C, after hydrolysate is added dropwise, and under the conditions of control reaction temperature is 80 ~ 90 DEG C, aging reaction 2h is carried out, with true
It is complete to protect aminating reaction, after aminating reaction, the temperature of charge in three-necked flask B is reduced to 70 ~ 80 DEG C, in constant pressure addition
Put into 67.5g deionized water and 67.5g alcohol mixeding liquid in funnel B, after stock, by constant pressure funnel B go from
Sub- water and alcohol mixeding liquid slowly, in uniform instillation three-necked flask B carry out the hydrolysis of 3- aminopropyl triethoxysilane,
It is 70 ~ 80 DEG C, after mixed liquor is added dropwise that reaction temperature is controlled in hydrolysis reaction, and control reaction temperature is 80 ~ 90 DEG C of items
Under part, aging reaction 2h is carried out, to ensure deionized water fully reacting, after, the temperature of charge in three-necked flask B is reduced
To 50 ~ 60 DEG C, 360g alcohol sodium solution is then put into constant pressure funnel B, and is slowly dropped into three-necked flask B in progress
It is reacted with dechlorination, temperature is controlled during neutralization reaction at 50-60 DEG C, after alcohol sodium solution is added dropwise, gradually three mouthfuls are burnt
Bottle B carries out heat temperature raising, and the ethyl alcohol in three-necked flask B is steamed, and after ethanol distillation, the material in three-necked flask B is dropped
Down to room temperature, then it is filtered to obtain the functional amino silane oligomer product of light-coloured transparent, low viscosity, low free chlorine.
Embodiment 3
182g throws chloropropylmethyldimethoxysilane and produces in the three-necked flask A for being connected with reflux condenser (logical down cycles water)
Product throw 13.5g deionized water, 27g methanol and 0.05g mixed in hydrochloric acid material in the constant pressure funnel A on connection three-necked flask,
After stock, magnetic stirring apparatus is opened, oil bath heating device is opened and leaks constant pressure addition after temperature of charge reaches 70 DEG C
The mixing of bucket A slowly, uniformly instills the hydrolysis of progress chloropropylmethyldimethoxysilane in three-necked flask A, water
Solving control reaction temperature in reaction process is 70 ~ 80 DEG C, after mixing is added dropwise, under the conditions of control reaction temperature is 80 ~ 90 DEG C,
Carry out aging reaction 2h, it is ensured that deionized water fully reacting, after, chloropropylmethyldimethoxysilane hydrolysate is down to
Room temperature.
1110gN-(2- aminoethyl is put into the three-necked flask B for being connected with reflux condenser (logical down cycles water)) -3- ammonia
Propyl trimethoxy silicane product throws chloropropyl dimethoxy silicon in the constant pressure funnel B on connection three-necked flask B
Alkane hydrolysate after stock, opens magnetic stirring apparatus, and opening oil bath heating device will be permanent after temperature of charge reaches 70 DEG C
The chloropropylmethyldimethoxysilane hydrolysate in dropping funel B is pressed slowly, in uniform instillation three-necked flask B to carry out chlorine third
Ylmethyl dimethoxysilane and N-(2- aminoethyl) -3- aminopropyl trimethoxysilane aminating reaction, by amino silane
H atom react away, it is 70 ~ 80 DEG C, after hydrolysate is added dropwise that reaction temperature is controlled during aminating reaction, control reaction temperature
Under the conditions of degree is 80 ~ 90 DEG C, aging reaction 2h is carried out, it is ensured that aminating reaction is complete, after, by the material in three-necked flask B
Temperature is reduced to 70 ~ 80 DEG C, throws 67.5g deionized water in constant pressure funnel B and 67.5g methyl alcohol mixed liquor, stock finish
Afterwards, by constant pressure funnel B deionized water and methyl alcohol mixed liquor slowly, uniform instill in three-necked flask B carry out N-(2-
Aminoethyl) -3- aminopropyl trimethoxysilane hydrolysis, control reaction temperature is 70 ~ 80 DEG C in hydrolysis reaction, is mixed
After conjunction liquid is added dropwise, under the conditions of control reaction temperature is 80 ~ 90 DEG C, aging reaction 2h is carried out, it is ensured that deionized water has been reacted
Entirely, after, the material in three-necked flask B is reduced to 50 ~ 60 DEG C, 195g sodium methoxide is then thrown in constant pressure funnel B
Solution, and be slowly dropped into three-necked flask B and neutralize dechlorination reaction, 50-60 DEG C of kettle temperature is controlled during neutralization reaction, methanol
After sodium solution is added dropwise, heat temperature raising gradually is carried out to three-necked flask B, the methanol in three-necked flask B is steamed, methanol distillation
After, the material in three-necked flask B is reduced to room temperature, is then filtered to obtain light-coloured transparent, low viscosity, low free chlorine
Functional amino silane oligomer product.
Claims (1)
1. a kind of preparation method of functionality amino silane oligomer, it is characterised in that: it the following steps are included:
1) chloropropyl alkoxy silane product, is added in the three-necked flask A for being connected with reflux condenser, in connection three-necked flask A
Constant pressure funnel A in the mixed liquor of deionized water, solvent and hydrochloric acid, wherein chloropropyl alkoxy silane and deionization is added
The molar ratio of water is 0.75, and the mass ratio of solvent and deionized water is 1:2.0, and hydrochloric acid additional amount is chloropropyl alkoxyl silicone
The 0.03% of alkane inventory；
2) after, stocking up, magnetic stirring apparatus is opened, oil bath heating device is opened, after temperature of charge reaches 70 DEG C, by constant pressure
The mixing of dropping funel A slowly, in uniform instillation three-necked flask A carries out the hydrolysis of chloropropyl alkoxy silane, hydrolysis
It is 70 ~ 80 DEG C that reaction temperature is controlled in reaction process；
3) after, mixing is added dropwise, under the conditions of control reaction temperature is 80 ~ 90 DEG C, aging reaction 2h is carried out, to ensure deionization
Water fully reacting, after, chloropropyl alkoxy silane hydrolysate is down to room temperature；
4) amino silane product, is thrown in the three-necked flask B for being connected with reflux condenser, in the constant pressure addition of connection three-necked flask B
Chloropropyl alkoxy silane hydrolysate is put into funnel B, wherein the molar ratio of amino silane and chloropropyl alkoxy silane is
1:0.1~0.3；
5) after feeding intake, magnetic stirring apparatus is opened, oil bath heating device is opened, after temperature of charge reaches 70 DEG C, by constant pressure addition
Chloropropyl alkoxy silane in funnel B slowly, in uniform instillation three-necked flask B carries out chloropropyl alkoxy silane and amino
The aminating reaction of silane, the H atom of amino silane is reacted away, and it is 70 ~ 80 DEG C that reaction temperature is controlled during aminating reaction；
6) after hydrolysate is added dropwise, under the conditions of control reaction temperature is 80 ~ 90 DEG C, aging reaction 2h is carried out, to ensure amination
Fully reacting, after, the temperature of charge in three-necked flask B is reduced to 70 ~ 80 DEG C；
7) deionized water and solvent mixed liquor are thrown in constant pressure funnel B, wherein the mass ratio of deionized water and solvent is
The molar ratio of 1:1, deionized water and amino silane is 0.75；
8) after stocking up, the deionized water mixed liquor in constant pressure funnel B slowly, is uniformly instilled in three-necked flask B
The hydrolysis of amino silane is carried out, control reaction temperature is 70 ~ 80 DEG C in hydrolysis reaction；
9) after mixed liquor is added dropwise, control reaction temperature be 80 ~ 90 DEG C under the conditions of, carry out aging reaction 2h, with ensure from
Sub- water fully reacting, after, the temperature of charge in three-necked flask B is reduced to 50 ~ 60 DEG C；
10) after aging reaction, suitable alcohol sodium solution is put into constant pressure funnel B, is then slowly dropped into three mouthfuls of burnings
It carries out neutralizing dechlorination reaction in bottle B, controls 50-60 DEG C of temperature during neutralization reaction；
11) after alcohol sodium solution is added dropwise, heat temperature raising gradually is carried out to three-necked flask B, the solvent in three-necked flask B is steamed
Out, solvent distillation after, the material in three-necked flask B is reduced to room temperature, is then filtered, obtains, light color, low viscosity,
The functional amino silane oligomer product of low free chlorine；
The solvent is methanol or ethyl alcohol；
The chloropropyl alkoxy silane product is r-chloropropyl trimethoxyl silane or chloropropyl triethoxysilane or chlorine
Hydroxypropyl methyl dimethoxysilane；
The amino silane is 3- aminopropyl trimethoxysilane or 3- aminopropyl triethoxysilane or N-(2- ammonia second
Base) -3- aminopropyl trimethoxysilane product.
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| CN110204727A (en) * | 2019-06-25 | 2019-09-06 | 荆州市江汉精细化工有限公司 | A kind of preparation method containing epoxy group and vinyl-silane-copolymer |
| CN112430245A (en) * | 2020-11-24 | 2021-03-02 | 江西晨光新材料股份有限公司 | Synthesis system and synthesis method of silicon nitrogen heterocyclic aminosilane |
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| CN112430245B (en) * | 2020-11-24 | 2023-03-03 | 江西晨光新材料股份有限公司 | Synthesis system and synthesis method of silicon nitrogen heterocyclic aminosilane |
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Application publication date: 20190517 |