CN109180719A - A kind of liquid alkaline prepares the technique and production system of silicon 69 - Google Patents
A kind of liquid alkaline prepares the technique and production system of silicon 69 Download PDFInfo
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- CN109180719A CN109180719A CN201811021019.9A CN201811021019A CN109180719A CN 109180719 A CN109180719 A CN 109180719A CN 201811021019 A CN201811021019 A CN 201811021019A CN 109180719 A CN109180719 A CN 109180719A
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- 239000007788 liquid Substances 0.000 title claims abstract description 48
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 34
- 239000010703 silicon Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 22
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- 238000000746 purification Methods 0.000 claims abstract description 22
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000003054 catalyst Substances 0.000 claims abstract description 16
- 239000005864 Sulphur Substances 0.000 claims abstract description 15
- 239000012043 crude product Substances 0.000 claims abstract description 15
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000003729 cation exchange resin Substances 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 11
- KSCAZPYHLGGNPZ-UHFFFAOYSA-N 3-chloropropyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)CCCCl KSCAZPYHLGGNPZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000003825 pressing Methods 0.000 claims abstract description 9
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 8
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 4
- 238000004042 decolorization Methods 0.000 claims description 4
- 229910000077 silane Inorganic materials 0.000 claims description 4
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 4
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 claims description 4
- 239000011593 sulfur Substances 0.000 claims description 3
- 229910052717 sulfur Inorganic materials 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 2
- 239000000460 chlorine Substances 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- -1 that is Substances 0.000 claims 2
- 150000001768 cations Chemical class 0.000 claims 1
- 239000011347 resin Substances 0.000 claims 1
- 229920005989 resin Polymers 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 7
- 239000000047 product Substances 0.000 abstract description 7
- 231100001261 hazardous Toxicity 0.000 abstract description 3
- 231100000614 poison Toxicity 0.000 abstract description 3
- 230000007096 poisonous effect Effects 0.000 abstract description 3
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 3
- 239000007822 coupling agent Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 125000003368 amide group Chemical class 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 125000000864 peroxy group Chemical group O(O*)* 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- TZRXHJWUDPFEEY-UHFFFAOYSA-N Pentaerythritol Tetranitrate Chemical group [O-][N+](=O)OCC(CO[N+]([O-])=O)(CO[N+]([O-])=O)CO[N+]([O-])=O TZRXHJWUDPFEEY-UHFFFAOYSA-N 0.000 description 1
- LNENVNGQOUBOIX-UHFFFAOYSA-N azidosilane Chemical class [SiH3]N=[N+]=[N-] LNENVNGQOUBOIX-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012954 diazonium Substances 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-O diazynium Chemical compound [NH+]#N IJGRMHOSHXDMSA-UHFFFAOYSA-O 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 1
- 239000011152 fibreglass Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000003444 phase transfer catalyst Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- HYHCSLBZRBJJCH-UHFFFAOYSA-N sodium polysulfide Chemical compound [Na+].S HYHCSLBZRBJJCH-UHFFFAOYSA-N 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
- C07F7/1872—Preparation; Treatments not provided for in C07F7/20
- C07F7/1892—Preparation; Treatments not provided for in C07F7/20 by reactions not provided for in C07F7/1876 - C07F7/1888
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/20—Purification, separation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses techniques and production system that a kind of liquid alkaline prepares silicon 69.Liquid alkaline, sulphur piece, solvent are added in reaction kettle, then heating stirring cools down, catalyst and chloropropyl triethoxysilane is added, obtains silane coupling agent crude product；Silane coupling agent crude product is decolourized by cation exchange resin；Solution after decoloration is filtered into purification kettle；Purification kettle is passed through steam, and filters pressing obtains silane coupling agent liquid i.e. silicon 69.The present invention optimizes equipment production flow, using synthesis, decoloration, purification, is granulated mode, and preparation process conditional is mild, easy to operate, in preparation process mainly based on liquid alkaline, does not add poisonous and hazardous organic solution, is easy for industrialized production；Formula is improved, is matched by the purifying of multi-process, produces product purity height.
Description
Technical field
The invention belongs to 69 production technology field of silicon, specially a kind of liquid alkaline prepares the technique and production system of silicon 69.
Background technique
A primary raw material of the silane coupling agent as tire can be improved wearability applied to tire, reduce hysteresis quality, increase
Strong modulus improves adhesive property to greatest extent, improves performance of technical process, tread wear, hot crackability, carcass and filler
The adhesive property of adhesive property, tire cushion.High-performance is researched and developed, the silane coupling agent product of high-purity is always each factory
The important process of family develops high purity silane coupling agent product and plays significance to the fast development of tyre industry.
Silane coupling agent commercialized development since the last century 40's, joined carbon and DOW CORNING by the U.S. before and after 1945
Equal companies develop and disclose a series of silane coupling agents with typical structure；Nineteen fifty-five UC company has been put forward for the first time containing amino
Silane coupling agent；Occur a series of modified amido silane coupling agents successively since nineteen fifty-nine；Phase early 1960s
The silane coupling agent with diazonium and nitrine structure that the silane coupling agent containing peroxy occurred and the latter stage sixties occur, but it is big
The kind of silane coupling agent is enriched greatly.In recent decades, with fiberglass reinforced plastics industrial expansion, various coupling agents
Research and development further speed up, modified amido silane coupling agent, peroxy silane coupling agent and azido silanes coupling agent
Synthesis and application all be this period main achievement.
Double-[γ-(triethoxysilicane) propyl] tetrasulfide (silicon 69) is one of silane coupled agent series products, is answered
Wearability can be improved for tire, improve performance of technical process.
The existing method for preparing silane coupling agent mainly has metallic sodium and the synthesis sodium polysulfide method of sulphur in the molten state
With the synthetic method etc. of piece alkali and sulphur in water phase.There is complicated for operation, reaction in the method for both synthesizing silane couplers
The disadvantages of process hazard, higher cost, yield are lower, are dfficult to apply to industrialize, and impurity is more, and purity is lower.
Summary of the invention
The present invention provides the technique and production system that a kind of liquid alkaline prepares silicon 69 aiming at above-mentioned defect.This
Invention optimization equipment production flow using synthesis, decoloration, purification, is granulated mode, and preparation process conditional is mild, easy to operate,
In preparation process mainly based on liquid alkaline, poisonous and hazardous organic solution is not added, is easy for industrialized production；Formula is improved,
It is matched by the purifying of multi-process, produces product purity height.
A kind of liquid alkaline of the invention prepares the technique of silicon 69 and production system technical solution is, a kind of liquid alkaline prepares silicon 69
Silicon 69 is prepared by synthesis, decoloration, purification in technique, comprising the following steps:
(1) it synthesizes: liquid alkaline, sulphur piece, solvent is added in reaction kettle, then heating stirring cools down, catalyst and chlorine is added
Propyl-triethoxysilicane obtains silane coupling agent crude product；
(2) physical decolorization: silane coupling agent crude product is decolourized by cation exchange resin；Solution after decoloration is filtered to mentioning
In pure kettle；
(3) purify: purification kettle is passed through steam, and filters pressing obtains silane coupling agent liquid i.e. silicon 69.
In step (1), liquid alkali: sulphur piece: catalyst: chloropropyl triethoxysilane=1.6 cubic metre: 680kg:
25kg:2 tons, the catalyst is tetrabutylammonium bromide.
In step (1), the liquid alkaline measured is added in reaction kettle, the sulphur piece of sulfur content 99.5% is then added, adds
Enter water and make solvent, heating stirring starts timing when the solution in reaction kettle is warming up to 100 DEG C, continues heating stirring and keeps shape
Then reaction solution is cooled to 80 degree by state 4h, catalyst is added, and chloropropyl triethoxysilane is added dropwise, and keeps the temperature 2.5h；It generates
Reaction solution is cooled to 50 degree of water phase layerings, lower clear liquid is separated, remaining liq is silane coupling agent crude product.
In step (2), the weight ratio of cation exchange resin decoloration and crude product is 1:5.
In step (2), after silane coupling agent crude product is mixed with cation exchange resin, it is heated to 45-50 DEG C, wherein not wrapping
50 DEG C are included, and stirs 1h, is then filtered, decolorising agent cation exchange resin is filtered out.
In step (3), purifying and be slowly introducing steam in kettle, pressure controls more than -0.09Mpa, and temperature rises to 100 degree,
1h is kept the temperature, is cooled to 50 degree hereinafter, filters pressing obtains silane coupling agent liquid i.e. silicon 69.
A kind of liquid alkaline prepares the production system of silicon 69, including sequentially connected reaction kettle, decoloration kettle, purification kettle, described
Reaction kettle is also connect with liquid caustic soda tank and catalyst tank, and reaction kettle is additionally provided with sulphur piece and chloropropyl triethoxysilane is added
Mouthful.
It is provided with the first lautertuns between reaction kettle and decoloration kettle, decolourizes to be provided with the second filtering between kettle and purification kettle
Slot.
Steam, which is provided with, on the purification kettle is passed through mouth.
Purification kettle discharge port is connect with filter-pressing device.
The invention has the benefit that the present invention solves complicated for operation, reagent consumption in the preparation of conventional silanes coupling agent
Greatly, higher cost, yield are lower, are dfficult to apply to the disadvantages of industrialization.Concentration is promoted simultaneously, solves in tire and wears no resistance
The problem of, reduce production cost.It is specific as follows:
1, using the synthetic reaction of chloropropyl triethoxysilane and liquid alkaline and sulphur piece, raw materials for production are both saved, are reduced
Entreprise cost, and improve product yield；
2, double-[γ-(three ethoxies are synthesized using ionized water and tetrabutylammonium bromide as reaction dissolvent and phase transfer catalyst respectively
Base silicon) propyl] tetrasulfide, it had not only solved the problems, such as the reaction of solid-liquid two-phase, but also improve reaction speed and yield, and had reduced enterprise
The production cost of industry；
3, the decolorising agent using cation exchange tree as double-[γ-(triethoxysilicane) propyl] tetrasulfide, does not pass through activity
Carbon decoloring improves the content and purity of double-[γ-(triethoxysilicane) propyl] tetrasulfide；
4, optimize equipment production flow, using synthesis, decoloration, purification, be granulated mode, preparation process conditional is mild, operation letter
Just；
5, in preparation process mainly based on liquid alkaline, poisonous and hazardous organic solution is not added, industrialized production is easy for；
6, formula is improved, is matched by the purifying of multi-process, produces product purity height.
69 component target of silicon that the present invention prepares is as shown in table 1:
Table 1
Detailed description of the invention:
Fig. 1 show operation system structure schematic diagram of the invention.
In figure, 1. liquid caustic soda tanks, 2. catalyst tanks, 3. reaction kettles, 4. first lautertuns, 5. decoloration kettles, 6. second lautertuns,
7. purifying kettle.
Specific embodiment:
For a better understanding of the present invention, below with specific example come the technical solution that the present invention will be described in detail, but it is of the invention
It is not limited thereto.
Embodiment 1
A kind of liquid alkaline prepares the technique of silicon 69, and silicon 69 is prepared by synthesis, decoloration, purification, comprising the following steps:
(1) it synthesizes: the liquid alkaline measured is added in reaction kettle 3, the sulphur piece of sulfur content 99.5% is then added, water is added
Solvent is made, heating stirring starts timing when the solution in reaction kettle 3 is warming up to 100 DEG C, continues heating stirring hold mode
Then reaction solution is cooled to 80 degree by 4h, catalyst is added, and chloropropyl triethoxysilane is added dropwise, and keeps the temperature 2.5h；What is generated is anti-
It answers liquid to be cooled to 50 degree of water phase layerings, lower clear liquid is separated, remaining liq is silane coupling agent crude product.Liquid alkali: sulphur piece:
Catalyst: chloropropyl triethoxysilane=1.6 cubic metre: 680kg:25kg:2 tons, the catalyst is tetrabutylammonium bromide.
(2) physical decolorization: after silane coupling agent crude product is mixed with cation exchange resin, being heated to 45-50 DEG C, wherein
Do not include 50 DEG C, and stir 1h, be then filtered, decolorising agent cation exchange resin is filtered out, solution is filtered to mentioning
In pure kettle 7.The weight ratio of cation exchange resin decoloration and crude product is 1:5.
(3) it purifying: being slowly introducing steam in purification kettle 7, pressure controls more than -0.09Mpa, and temperature rises to 100 degree,
1h is kept the temperature, is cooled to 50 degree hereinafter, filters pressing obtains silane coupling agent liquid i.e. silicon 69.
69 component target of silicon prepared is as shown in table 1:
Table 1
Embodiment 2
A kind of liquid alkaline prepares the production system of silicon 69, including sequentially connected reaction kettle 3, the first lautertuns 4, decoloration kettle 5, second
Lautertuns 6, purification kettle 7, the reaction kettle 3 are also connect with liquid caustic soda tank 1 and catalyst tank 2, and reaction kettle 3 is additionally provided with sulphur piece
Mouth is added with chloropropyl triethoxysilane.
Steam, which is provided with, on the purification kettle 7 is passed through mouth.
Purification 7 discharge port of kettle is connect with filter-pressing device.
Claims (10)
1. the technique that a kind of liquid alkaline prepares silicon 69, which is characterized in that silicon 69 is prepared by synthesis, decoloration, purification, including with
Lower step:
(1) it synthesizes: liquid alkaline, sulphur piece, solvent is added in reaction kettle, then heating stirring cools down, catalyst and chlorine is added
Propyl-triethoxysilicane obtains silane coupling agent crude product；
(2) physical decolorization: silane coupling agent crude product is decolourized by cation exchange resin；Solution after decoloration is filtered to mentioning
In pure kettle；
(3) purify: purification kettle is passed through steam, and filters pressing obtains silane coupling agent liquid i.e. silicon 69.
2. the technique that a kind of liquid alkaline according to claim 1 prepares silicon 69, which is characterized in that in step (1), liquid alkali:
Sulphur piece: catalyst: chloropropyl triethoxysilane=1.6 cubic metre: 680kg:25kg:2 tons, the catalyst is the tetrabutyl
Ammonium bromide.
3. the technique that a kind of liquid alkaline according to claim 1 prepares silicon 69, which is characterized in that in step (1), will measure
Liquid alkaline be added reaction kettle in, then be added sulfur content 99.5% sulphur piece, be added water do solvent, heating stirring, wait react
Solution in kettle starts timing when being warming up to 100 DEG C, continue heating stirring hold mode 4h, reaction solution is then cooled to 80
Catalyst is added in degree, and chloropropyl triethoxysilane is added dropwise, and keeps the temperature 2.5h；The reaction solution of generation is cooled to 50 degree of water phase layerings,
Lower clear liquid is separated, remaining liq is silane coupling agent crude product.
4. the technique that a kind of liquid alkaline according to claim 1 prepares silicon 69, which is characterized in that in step (2), cation is handed over
The weight ratio for changing resin decolorization and crude product is 1:5.
5. the technique that a kind of liquid alkaline according to claim 1 prepares silicon 69, which is characterized in that silane coupled in step (2)
After agent crude product is mixed with cation exchange resin, it is heated to 45-50 DEG C, wherein not including 50 DEG C, and 1h is stirred, then carried out
Filter, filters out decolorising agent cation exchange resin.
6. the technique that a kind of liquid alkaline according to claim 1 prepares silicon 69, which is characterized in that in step (3), purify in kettle
It is slowly introducing steam, pressure controls more than -0.09Mpa, and temperature rises to 100 degree, keeps the temperature 1h, is cooled to 50 degree hereinafter, filters pressing
Obtain silane coupling agent liquid, that is, silicon 69.
7. the production system that a kind of liquid alkaline prepares silicon 69, which is characterized in that including sequentially connected reaction kettle, decoloration kettle, purification
Kettle, the reaction kettle are also connect with liquid caustic soda tank and catalyst tank, and reaction kettle is additionally provided with sulphur piece and chloropropyl triethoxy
Mouth is added in silane.
8. the production system that a kind of liquid alkaline according to claim 7 prepares silicon 69, which is characterized in that reaction kettle and decoloration kettle
Between be provided with the first lautertuns, decolourize to be provided with the second lautertuns between kettle and purification kettle.
9. the production system that a kind of liquid alkaline according to claim 7 prepares silicon 69, which is characterized in that on the purification kettle
It is provided with steam and is passed through mouth.
10. the production system that a kind of liquid alkaline according to claim 7 prepares silicon 69, which is characterized in that purification kettle discharge port
It is connect with filter-pressing device.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811021019.9A CN109180719A (en) | 2018-09-03 | 2018-09-03 | A kind of liquid alkaline prepares the technique and production system of silicon 69 |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811021019.9A CN109180719A (en) | 2018-09-03 | 2018-09-03 | A kind of liquid alkaline prepares the technique and production system of silicon 69 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112047975A (en) * | 2020-09-02 | 2020-12-08 | 山东阳谷华泰化工股份有限公司 | Synthesis method of silane coupling agent Si69 and intermediate thereof |
| CN112694498A (en) * | 2020-12-30 | 2021-04-23 | 江西晨光新材料股份有限公司 | Naphthylamine-containing sulfur-containing silane and preparation method and application thereof |
| CN113278028A (en) * | 2020-02-19 | 2021-08-20 | 新特能源股份有限公司 | Method and equipment for preparing bis- [ gamma- (triethoxysilyl) propyl ] tetrasulfide |
| CN114699800A (en) * | 2022-03-23 | 2022-07-05 | 国家能源集团新疆能源有限责任公司 | Method for purifying Si69 stock solution |
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| US20040092758A1 (en) * | 2002-11-12 | 2004-05-13 | Buesing Chad Aaron | Method of making sulfur containing organosilicon compounds |
| CN103073569A (en) * | 2013-02-05 | 2013-05-01 | 景德镇宏柏化学科技有限公司 | Production process of organosilane polysulfide |
| CN103788121A (en) * | 2014-01-28 | 2014-05-14 | 南京曙光硅烷化工有限公司 | Method for producing light-color polysulfide silane coupling agent without buffer agent |
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2018
- 2018-09-03 CN CN201811021019.9A patent/CN109180719A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040092758A1 (en) * | 2002-11-12 | 2004-05-13 | Buesing Chad Aaron | Method of making sulfur containing organosilicon compounds |
| CN103073569A (en) * | 2013-02-05 | 2013-05-01 | 景德镇宏柏化学科技有限公司 | Production process of organosilane polysulfide |
| CN103788121A (en) * | 2014-01-28 | 2014-05-14 | 南京曙光硅烷化工有限公司 | Method for producing light-color polysulfide silane coupling agent without buffer agent |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113278028A (en) * | 2020-02-19 | 2021-08-20 | 新特能源股份有限公司 | Method and equipment for preparing bis- [ gamma- (triethoxysilyl) propyl ] tetrasulfide |
| CN113278028B (en) * | 2020-02-19 | 2022-12-20 | 新特能源股份有限公司 | Method and equipment for preparing bis- [ gamma- (triethoxysilyl) propyl ] tetrasulfide |
| CN112047975A (en) * | 2020-09-02 | 2020-12-08 | 山东阳谷华泰化工股份有限公司 | Synthesis method of silane coupling agent Si69 and intermediate thereof |
| CN112047975B (en) * | 2020-09-02 | 2023-09-05 | 山东阳谷华泰化工股份有限公司 | Synthesis method of silane coupling agent Si69 and intermediate thereof |
| CN112694498A (en) * | 2020-12-30 | 2021-04-23 | 江西晨光新材料股份有限公司 | Naphthylamine-containing sulfur-containing silane and preparation method and application thereof |
| CN114699800A (en) * | 2022-03-23 | 2022-07-05 | 国家能源集团新疆能源有限责任公司 | Method for purifying Si69 stock solution |
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