CN103833783B - The method of dibutyltindilaurate catalyzed synthesizing methoxy oximinoketone base silane - Google Patents
The method of dibutyltindilaurate catalyzed synthesizing methoxy oximinoketone base silane Download PDFInfo
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- CN103833783B CN103833783B CN201410066343.8A CN201410066343A CN103833783B CN 103833783 B CN103833783 B CN 103833783B CN 201410066343 A CN201410066343 A CN 201410066343A CN 103833783 B CN103833783 B CN 103833783B
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- oximinoketone
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Abstract
A kind of method that the invention discloses dibutyltindilaurate catalyzed synthesizing methoxy oximinoketone base silane, relate to cross-linking agent field, comprise the following steps: by mass parts, 1 part of tetramethoxy-silicane, 0.2～2.5 part of diacetylmonoxime and 0.0005～0.005 part of dibutyl tin laurate are added the reactor with gas phase extraction device, under conditions of temperature in reactor is 121 DEG C～129 DEG C, stirring reaction 3～7h, obtains product to be distilled；It is 100 DEG C～120 DEG C in temperature, under conditions of pressure is 0.095～0.098MPa, treats distillage and distill, obtain methoxyl group oximinoketone base silane complex.The dibutyl tin laurate of the present invention can be as the catalyst of room temperature vulcanized silicone rubber molding, and after having reacted, dibutyl tin laurate can be retained in the reaction product, and reactions steps is fairly simple；The present invention uses tetramethoxy-silicane to be raw material, and synthesis cost is relatively low.
Description
Technical field
The present invention relates to cross-linking agent field, be specifically related to a kind of dibutyltindilaurate catalyzed conjunction
The method becoming methoxyl group oximinoketone base silane.
Background technology
Existing room temperature vulcanized silicone rubber, during curing molding, generally uses methyl three fourth
Ketoximinosilanes, four diacetylmonoxime base silanes, MTMS and oximinoketone ylmethoxy silicon
Alkane complex is as cross-linking agent, it is achieved the curing molding of room temperature vulcanized silicone rubber rubber cross.
When using methyl tributanoximo silane as cross-linking agent, the solidification of room temperature vulcanized silicone rubber
Shaping speed is slow；When using four diacetylmonoxime base silanes as cross-linking agent, due to four diacetylmonoxime
The freezing point of base silane is higher (about 40 DEG C), and during use, four diacetylmonoxime base silanes easily crystallize,
The curing molding speed causing room temperature vulcanized silicone rubber is difficult to control to, and the vulcanite obtained
Finished product is more crisp, and percentage elongation is poor；MTMS is used to synthesize as cross-linking agent
Room temperature vulcanized silicone rubber store time, less stable.
Methoxyl group diacetylmonoxime base silane complex is trimethoxy diacetylmonoxime base silane, dimethoxy
Two diacetylmonoxime base silanes, methoxyl group tributanoximo silane and the mixture of four diacetylmonoxime base silanes.
When methoxyl group diacetylmonoxime base silane complex is as cross-linking agent, being solidified into of room temperature vulcanized silicone rubber
Type expression activitiy is high, and curing rate ratio is very fast, uses more convenient, it is also possible to each by regulation
The content of component controls curing rate, and the room temperature vulcanized silicone rubber bin stability of synthesis compares
Good.
Existing synthesizing methoxy oximinoketone base silane complex method is: use chlorosilane, organic
Chlorosilane, diacetylmonoxime and methanol are raw material, at catalyst calcium chloride, butyl titanate and aminated
Under the catalysis of compound, lactate synthesis methoxyl group oximinoketone base silane complex.
But, there is following defect in existing synthesizing methoxy oximinoketone base silane complex method:
(1) using chlorosilane, organochlorosilane, diacetylmonoxime and methanol is raw material, metatitanic acid fourth
Ester is that the color of catalyst synthesizing methoxy oximinoketone base silane complex is relatively deep, methoxyl group oximinoketone base
Silane compound easily solidifies when using, and crosslinking active is relatively low.Catalyst calcium chloride is powder
Solid, remains after having reacted and is difficult in the reaction product remove.Amine compound and methoxyl group
The boiling point of oximinoketone base silane complex relatively, amine compound and methoxyl group oximinoketone base silane
Complex is difficult to separate；Owing to amine compound residual causes the crosslinking of synthesis in the reaction product
Agent crosslinking active is relatively low, and remains the product of amino-compound and long-time storage
After, easily turn yellow.
(2) methoxyl group oximinoketone base silane complex uses chlorosilane, organochlorosilane to be raw material,
Chlorosilane and organochlorosilane reaction can produce hydrogen chloride gas, and hydrogen chloride gas pollutes the environment,
The certain hidden danger of security presence.
Summary of the invention
For defect present in prior art, it is an object of the invention to provide a kind of two Laurels
The method that acid dibutyl tin catalyzes and synthesizes methoxyl group oximinoketone base silane, synthesizing methoxy oximinoketone base silicon
The step of alkane complex is fairly simple, and the color ratio of product is shallower, and crosslinking active is higher,
Not only compare safety, and it is relatively low to synthesize cost ratio.
For reaching object above, the present invention adopts the technical scheme that: a kind of tin dilaurate two fourth
Ji Xi catalyzes and synthesizes the method for methoxyl group oximinoketone base silane, it is characterised in that comprise the following steps:
A, by mass parts by 1 part of tetramethoxy-silicane, 0.2～2.5 part of diacetylmonoxime and 0.0005～
0.005 part of dibutyl tin laurate, adds the reactor with gas phase extraction device；Keep
The temperature of gas phase extraction mouth is below 76 DEG C, by tetramethoxy-silicane, diacetylmonoxime and two Laurels
After acid dibutyl tin is warming up to 121 DEG C～129 DEG C, stirs 3～7h, obtain product to be distilled；
B, temperature be 100～120 DEG C, pressure for-0.095～-0.098MPa under conditions of,
Treat distillage to distill, obtain methoxyl group oximinoketone base silane complex.
On the basis of technique scheme, step A keep the temperature of gas phase extraction mouth exist
76 DEG C of following steps included below: under conditions of the temperature of gas phase extraction mouth is 70 DEG C～75 DEG C,
Start gas extraction；Under conditions of the temperature of gas phase extraction mouth is 76 DEG C, reactor is entered
Row infinite reflux, persistently carries out gas extraction.
On the basis of technique scheme, step A comprises the following steps: by 1 part of tetramethyl
TMOS, 0.5～1 part of diacetylmonoxime and 0.0015～0.001 part of dibutyl tin laurate,
Add the reactor with gas phase extraction device；Keep gas phase extraction mouth temperature 76 DEG C with
Under, after tetramethoxy-silicane, diacetylmonoxime and dibutyl tin laurate are warming up to 125 DEG C,
Stirring 5h, obtains product to be distilled.
On the basis of technique scheme, described dibutyl tin laurate is 0.0025 part.
On the basis of technique scheme, described diacetylmonoxime is 0.25 part.
On the basis of technique scheme, by tetramethoxy-silicane, diacetylmonoxime in step A
It is warming up to 121 DEG C～129 DEG C with dibutyl tin laurate comprise the following steps: by methoxyl group
Silane, diacetylmonoxime and dibutyl tin laurate stirring are warming up to 121 DEG C～129 DEG C.
On the basis of technique scheme, described methoxyl group oximinoketone base silane complex includes four
Methoxy silane, trimethoxy diacetylmonoxime base silane, diacetylmonoxime, dimethoxy two butanone oximido
Silane and methoxyl group tributanoximo silane.
On the basis of technique scheme, in described methoxyl group oximinoketone base silane complex, four
The content of methoxy silane is 0.5%～5.5%, the content of fourth oximinoketone is 2.0%～5.2%, three
The content of methoxyl group diacetylmonoxime base silane is 12.5%～82.5%, dimethoxy two butanone oximido
The content of silane is 4.9%～30.3%, the content of methoxyl group tributanoximo silane be 0.5%～
33.8%, the content of four diacetylmonoxime base silanes is 0%～15.2%.
On the basis of technique scheme, the colourity of described methoxyl group oximinoketone base silane complex
Be 60～180 black once.
On the basis of technique scheme, the pH of described methoxyl group oximinoketone base silane complex
Value is 6～8.
Compared with prior art, it is an advantage of the current invention that:
(1) the catalyst dibutyltin dilaurylate of the present invention, can not only be catalyzed methoxyl group
The synthesis of oximinoketone base silane, and itself can be as room temperature vulcanized silicone rubber in curing molding process
In catalyst, therefore, after dibutyltindilaurate catalyzed synthesizing methoxy oximinoketone base silane,
Dibutyl tin laurate can directly be retained in the reaction product, and reactions steps is fairly simple,
Dibutyl tin laurate can dissolve each other with methoxyl group oximinoketone base silane, the color ratio of product
Shallower, the crosslinking active of product is higher.
(2) present invention uses tetramethoxy-silicane to be raw material, and tetramethoxy-silicane is trimethoxy
By-product in the synthesis of base hydrogen silane, uses fewer in industry, price comparison is low.The present invention
The most effectively alleviate overstocking of tetramethoxy-silicane, and it is relatively low to synthesize cost ratio.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail.
The dibutyltindilaurate catalyzed synthesizing methoxy oximinoketone base silane that the present invention provides is multiple
The method of compound, comprises the following steps: by mass parts by 1 part of tetramethoxy-silicane, 0.2～
2.5(is preferably 0.5～1 part) part diacetylmonoxime and 0.0005～0.005(be preferably 0.0025～
0.001 part) part dibutyl tin laurate adds with the reactor of gas phase extraction device, rises
Temperature reactor also detects the temperature of gas phase extraction mouth；Temperature at gas phase extraction mouth is 70 DEG C～75 DEG C
Under conditions of, carry out methanol gas extraction；The condition that temperature is 76 DEG C at gas phase extraction mouth
Lower beginning infinite reflux, keeps the temperature of gas phase extraction mouth below 76 DEG C, continues extraction methanol
Gas, is warming up to the stirring of tetramethoxy-silicane, diacetylmonoxime and dibutyl tin laurate
121 DEG C～129 DEG C, stirring reaction 3～7h, obtain product to be distilled, temperature be 100 DEG C～
120 DEG C, pressure for distilling product to be distilled under conditions of-0.095～-0.098MPa, obtain first
Epoxide oximinoketone base silane complex.
Reactor is the 1000ml being provided with agitator, reflux condensing tube, condensing tube and thermometer
There-necked flask, gas phase extraction device includes still head, condensing tube, connect tail pipe and volume is 500ml
Receiving flask.
Dibutyl tin laurate in the present invention acts not only as catalyst, and can make
For room temperture rubber vulcanization catalyst during curing molding, therefore two Laurels in the present invention
Acid dibutyl tin can directly be retained in the reaction product, and does not affect the use of product
Performance.
The pH value of methoxyl group oximinoketone base silane complex is 6～8, and methoxyl group oximinoketone base silane is multiple
Compound includes tetramethoxy-silicane, trimethoxy diacetylmonoxime base silane, diacetylmonoxime, dimethoxy
Two diacetylmonoxime base silanes and methoxyl group tributanoximo silane.
Methoxyl group oximinoketone base silane is analyzed by GC (Gas Chromatography gas chromatogram)
Complex, obtains in methoxyl group oximinoketone base silane complex, and the content of tetramethoxy-silicane is
0.5%～5.5%, the content of fourth oximinoketone be 2.0%～5.2%, trimethoxy diacetylmonoxime base silane
Content be 12.5%～82.5%, the content of dimethoxy two diacetylmonoxime base silane be 4.9%～
30.3%, the content of methoxyl group tributanoximo silane is 0.5%～33.8%, four butanone oximidos
The content of silane is 0%～15.2%, and other content is 2.5%～4.6%.
The reaction equation of the embodiment of the present invention is
(CH3O)3Si+C2H3C(NOH)CH3→CH3Si(OCH3)3+HON=C(CH3)(C2H5)→
CH3Si(OCH3)2ON=C(CH3)(C2H5)+CH3(OCH3)ON=C[(CH3)(C2H5)]2+C
H3Si[ON=C(CH3)(C2H5)]+CH3OH↑。
Use GB/T605-2006 chemical reagent determination of colority universal method to methoxyl group oximinoketone base
Silane compound is measured, obtain the colourity of methoxyl group oximinoketone base silane complex be 60～
180 black once.
Below, by 5 embodiments, the present invention is described in detail:
Embodiment 1
In the there-necked flask of 1000ml, add 500g tetramethoxy-silicane, 125g butanone
Oxime and 0.75g dibutyl tin laurate, there-necked flask with agitator, reflux condensing tube,
Gas phase extraction device and thermometer, heat up to there-necked flask and detect the temperature of gas phase extraction mouth
Degree, adopts when outlet temperature is 72 DEG C when gas phase and starts gas phase extraction, when gas phase adopts outlet temperature
It is when 76 DEG C, to start infinite reflux, keeps gas phase to adopt outlet temperature and be not higher than 76 DEG C and persistently extraction
Methanol gas, stirring reaction 2h under conditions of keeping the temperature in there-necked flask to be 121 DEG C,
To product to be distilled, being 100 DEG C in temperature, under conditions of pressure is-0.095Mp, distillation is treated
Distillage obtains methoxyl group oximinoketone base silane complex.
Empirical tests: the quality obtaining methoxyl group oximinoketone base silane complex is 225.2g, and colourity is
60 black once, pH is 6.
The composition being obtained methoxyl group oximinoketone base silane complex by GC analysis is as follows: methoxyl group
In oximinoketone base silane complex, the content of tetramethoxy-silicane is 1.3%, the content of diacetylmonoxime
Be 3.1%, the content of trimethoxy diacetylmonoxime base silane be 80.5%, dimethoxy two butanone
The content of oximino silane is 10.5%, the content of methoxyl group tributanoximo silane is 1.6%,
The content of four diacetylmonoxime base silanes is 0%, other content is 3.0%.
Embodiment 2
In the there-necked flask of 1000ml, add 500g tetramethoxy-silicane, 100g butanone
Oxime and 0.25g dibutyl tin laurate, there-necked flask with agitator, reflux condensing tube,
Gas phase extraction device and thermometer, heat up to there-necked flask and detect the temperature of gas phase extraction mouth
Degree, adopts when outlet temperature is 70 DEG C when gas phase and starts gas phase extraction, when gas phase adopts outlet temperature
It is when 76 DEG C, to start infinite reflux, keeps gas phase to adopt outlet temperature and be not higher than 76 DEG C and persistently extraction
Methanol gas, under conditions of the temperature in there-necked flask is 125 DEG C, 5h is reacted in stirring, obtains
Product to be distilled, is 115 DEG C in temperature, and under conditions of pressure is-0.096Mpa, distillation is treated
Distillage obtains methoxyl group oximinoketone base silane complex.
Empirical tests: the quality obtaining methoxyl group oximinoketone base silane complex is 210.3g, and colourity is
180 black once, pH is 7.
The composition being obtained methoxyl group oximinoketone base silane complex by GC analysis is as follows: methoxyl group
In oximinoketone base silane complex, the content of tetramethoxy-silicane is 5.5%, the content of diacetylmonoxime
Be 2.0%, the content of trimethoxy tributanoximo silane be 82.5%, dimethoxy two fourth
The content of ketoximinosilanes is 4.9%, the content of methoxyl group tributanoximo silane is 0.5%,
The content of four diacetylmonoxime base silanes is 0%, other content is 4.6%.
Embodiment 3
In the there-necked flask of 1000ml, add 200g tetramethoxy-silicane, 500g butanone
Oxime and 1g dibutyl tin laurate, there-necked flask be with agitator, reflux condensing tube,
Gas phase extraction device and thermometer, heat up to there-necked flask and detect the temperature of gas phase extraction mouth
Degree, adopts when outlet temperature is 75 DEG C when gas phase and starts gas phase extraction, when gas phase adopts outlet temperature
It is when 76 DEG C, to start infinite reflux, keeps gas phase to adopt outlet temperature and be not higher than 76 DEG C and persistently extraction
Methanol gas, under conditions of the temperature in there-necked flask is 129 DEG C, 7h is reacted in stirring, obtains
Product to be distilled, is 120 DEG C in temperature, and under conditions of pressure is-0.098Mpa, distillation is treated
Distillage obtains methoxyl group oximinoketone base silane complex.
Empirical tests: the quality obtaining methoxyl group oximinoketone base silane complex is 260g, and colourity is
65 black once, pH is 8.
The composition being obtained methoxyl group oximinoketone base silane complex by GC analysis is as follows: methoxyl group
In oximinoketone base silane complex, the content of tetramethoxy-silicane is 0.5%, the content of diacetylmonoxime
Be 5.2%, the content of trimethoxy tributanoximo silane be 12.5%, dimethoxy two fourth
The content of ketoximinosilanes is 30.3%, the content of methoxyl group tributanoximo silane is 33.8%,
The content of four diacetylmonoxime base silanes is 15.2%, other content is 2.5%.
Embodiment 4
In the there-necked flask of 1000ml, add 200g tetramethoxy-silicane, 200g butanone
Oxime and 0.2g dibutyl tin laurate, there-necked flask be with agitator, reflux condensing tube,
Gas phase extraction device and thermometer, heat up to there-necked flask and detect the temperature of gas phase extraction mouth
Degree, adopts when outlet temperature is 75 DEG C when gas phase and starts gas phase extraction, when gas phase adopts outlet temperature
It is when 76 DEG C, to start infinite reflux, keeps gas phase to adopt outlet temperature and be not higher than 76 DEG C and persistently extraction
Methanol gas, under conditions of the temperature in there-necked flask is 129 DEG C, 7h is reacted in stirring, obtains
Product to be distilled, is 120 DEG C in temperature, and under conditions of pressure is-0.098Mpa, distillation is treated
Distillage obtains methoxyl group oximinoketone base silane complex.
Empirical tests: the quality obtaining methoxyl group oximinoketone base silane complex is 240g, and colourity is
70 black once, pH is 8.
The composition being obtained methoxyl group oximinoketone base silane complex by GC analysis is as follows: methoxyl group
In oximinoketone base silane complex, the content of tetramethoxy-silicane is 1.2%, the content of diacetylmonoxime
Be 4.9%, the content of trimethoxy tributanoximo silane be 40.7%, dimethoxy two fourth
The content of ketoximinosilanes is 24.3%, the content of methoxyl group tributanoximo silane is 19.4%,
The content of four diacetylmonoxime base silanes is 6.2%, other content is 3.3%.
Embodiment 5
In the there-necked flask of 1000ml, add 500g tetramethoxy-silicane, 250g butanone
Oxime and 0.5g dibutyl tin laurate, there-necked flask be with agitator, reflux condensing tube,
Gas phase extraction device and thermometer, heat up to there-necked flask and detect the temperature of gas phase extraction mouth
Degree, adopts when outlet temperature is 75 DEG C when gas phase and starts gas phase extraction, when gas phase adopts outlet temperature
It is when 76 DEG C, to start infinite reflux, keeps gas phase to adopt outlet temperature and be not higher than 76 DEG C and persistently extraction
Methanol gas, under conditions of the temperature in there-necked flask is 129 DEG C, 3h is reacted in stirring, obtains
Product to be distilled, is 120 DEG C in temperature, and under conditions of pressure is-0.098Mpa, distillation is treated
Distillage obtains methoxyl group oximinoketone base silane complex.
Empirical tests: the quality obtaining methoxyl group oximinoketone base silane complex is 230g, and colourity is
62 black once, pH is 6.
The composition being obtained methoxyl group oximinoketone base silane complex by GC analysis is as follows: methoxyl group
In oximinoketone base silane complex, the content of tetramethoxy-silicane is 1.5%, the content of diacetylmonoxime
Be 4.5%, the content of trimethoxy tributanoximo silane be 60.7%, dimethoxy two fourth
The content of ketoximinosilanes is 18.3%, the content of methoxyl group tributanoximo silane is 9.7%,
The content of four diacetylmonoxime base silanes is 2.6%, other content is 2.7%.
The present invention is not limited to above-mentioned embodiment, for those skilled in the art
For, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications,
Within these improvements and modifications are also considered as protection scope of the present invention.This specification is not made in detail
The content described belongs to prior art known to professional and technical personnel in the field.
Claims (10)
1. a method for dibutyltindilaurate catalyzed synthesizing methoxy oximinoketone base silane,
It is characterized in that, comprise the following steps:
A, by mass parts by 1 part of tetramethoxy-silicane, 0.2～2.5 part of diacetylmonoxime and 0.0005～
0.005 part of dibutyl tin laurate, adds the reactor with gas phase extraction device；Keep
The temperature of gas phase extraction mouth is below 76 DEG C, by tetramethoxy-silicane, diacetylmonoxime and two Laurels
After acid dibutyl tin is warming up to 121 DEG C～129 DEG C, stirs 3～7h, obtain product to be distilled；
B, temperature be 100～120 DEG C, pressure for-0.095～-0.098MPa under conditions of,
Treat distillage to distill, obtain methoxyl group oximinoketone base silane complex.
Dibutyltindilaurate catalyzed synthesizing methoxy oximinoketone the most as claimed in claim 1
The method of base silane, it is characterised in that keep the temperature of gas phase extraction mouth at 76 DEG C in step A
Following steps included below: under conditions of the temperature of gas phase extraction mouth is 70 DEG C～75 DEG C, open
Beginning gas extraction；Under conditions of the temperature of gas phase extraction mouth is 76 DEG C, reactor is carried out
Infinite reflux, persistently carries out gas extraction.
Dibutyltindilaurate catalyzed synthesizing methoxy oximinoketone the most as claimed in claim 1
The method of base silane, it is characterised in that step A comprises the following steps: by 1 part of four methoxy
Base silane, 0.5～1 part of diacetylmonoxime and 0.0015～0.001 part of dibutyl tin laurate, add
Enter the reactor with gas phase extraction device；Keep gas phase extraction mouth temperature below 76 DEG C,
After tetramethoxy-silicane, diacetylmonoxime and dibutyl tin laurate are warming up to 125 DEG C, stirring
5h, obtains product to be distilled.
Dibutyltindilaurate catalyzed synthesizing methoxy oximinoketone the most as claimed in claim 3
The method of base silane, it is characterised in that: described dibutyl tin laurate is 0.0025 part.
Dibutyltindilaurate catalyzed synthesizing methoxy oximinoketone the most as claimed in claim 1
The method of base silane, it is characterised in that: described diacetylmonoxime is 0.25 part.
Dibutyltindilaurate catalyzed synthesizing methoxy oximinoketone the most as claimed in claim 1
The method of base silane, it is characterised in that in step A by tetramethoxy-silicane, diacetylmonoxime and
Dibutyl tin laurate is warming up to 121 DEG C～129 DEG C and comprises the following steps: by methoxyl group silicon
Alkane, diacetylmonoxime and dibutyl tin laurate stirring are warming up to 121 DEG C～129 DEG C.
Dibutyltindilaurate catalyzed synthesizing methoxy oximinoketone the most as claimed in claim 1
The method of base silane, it is characterised in that: described methoxyl group oximinoketone base silane complex includes tetramethyl
TMOS, trimethoxy diacetylmonoxime base silane, diacetylmonoxime, dimethoxy two butanone oximido silicon
Alkane and methoxyl group tributanoximo silane.
Dibutyltindilaurate catalyzed synthesizing methoxy oximinoketone the most as claimed in claim 7
The method of base silane, it is characterised in that: in described methoxyl group oximinoketone base silane complex, tetramethyl
The content of TMOS is 0.5%～5.5%, the content of fourth oximinoketone is 2.0%～5.2%, front three
The content of epoxide diacetylmonoxime base silane is 12.5%～82.5%, dimethoxy two butanone oximido silicon
The content of alkane is 4.9%～30.3%, the content of methoxyl group tributanoximo silane be 0.5%～
33.8%, the content of four diacetylmonoxime base silanes is 0%～15.2%.
Dibutyltindilaurate catalyzed synthesizing methoxy oximinoketone the most as claimed in claim 1
The method of base silane, it is characterised in that: the colourity of described methoxyl group oximinoketone base silane complex is
60～180 black once.
Dibutyltindilaurate catalyzed synthesizing methoxy oximinoketone the most as claimed in claim 1
The method of base silane, it is characterised in that: the pH value of described methoxyl group oximinoketone base silane complex
It is 6～8.
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