CN201722313U - Double-propyltriethoxysilane four-sulfide distillation apparatus - Google Patents
Double-propyltriethoxysilane four-sulfide distillation apparatus Download PDFInfo
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- CN201722313U CN201722313U CN2010201539863U CN201020153986U CN201722313U CN 201722313 U CN201722313 U CN 201722313U CN 2010201539863 U CN2010201539863 U CN 2010201539863U CN 201020153986 U CN201020153986 U CN 201020153986U CN 201722313 U CN201722313 U CN 201722313U
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Abstract
The utility model discloses a double-propyltriethoxysilane four-sulfide distillation apparatus, which comprises a distillation kettle, a distillation tower, a condenser and a receiving tank. The distillation tower includes a bottom tower section, a middle tower section and an upper tower section, and a lower return flow short section and an upper return flow short section are respectively arranged between the bottom tower section and the middle tower section and between the middle tower section and the upper tower section. The double-propyltriethoxysilane four-sulfide distillation apparatus adopts a double-return-flow adjusting gas-liquid double-phase material composition, can adjust return flow ratio according to changes of purity of products in the return tank, improves distillation effect and purity of distillation products by reaching more than 98% (GC), reduces distillation residues with product impurity content lower than or equal to 1% (GC), simultaneously improves product yield, and enlarges application field of the products.
Description
Technical field
The utility model relates to the chemical industry equipment field, relates in particular to a kind of pair-[propyl-triethoxysilicane]-tetrasulfide water distilling apparatus.
Background technology
Two-[propyl-triethoxysilicane]-tetrasulfide (are called for short Si-69) are a kind ofly to have crosslinked in rubber item and many sulphur of the bifunctional organo silane coupling agent active catalytic effect.Si-69 is mainly used in rubber industry, it not only has the effect of activator, coupling agent, the effect that also has linking agent, tenderizer and strengthening agent, can significantly reduce the viscosity of white carbon black and rubber combined material, give the rubber good processing properties, particularly can avoid the cured natural rubber material phenomenon of reverting.Si-69 is not only applicable to natural gum, isoamyl glue, butadiene-styrene rubber, cis-butadiene cement, butadiene-acrylonitrile rubber, neoprene latex, butyl and halogenated butyl glue, ethylene-propylene diene copolymer, is applicable to the blended rubber material of these rubber yet; Also can be used for making tire tread, sidewall, carcass static and that dynamic condition uses down, steel wire adhesive material, transmission belt outer layer glue, solid tyre, cable insulation and coating material, rubber roll and sole or the like, particularly light-colour rubber goods.The main effect of Si-69 is to improve Young's modulus, tensile strength and the tearing toughness of rubber, significantly improves the wear resisting property and the compression performance of rubber; Reduce the permanent modification of rubber; Reduce rubber viscosity, save power consumption of polymer processing.
The production of chemical industry Si-69 at present mainly contains two kinds of methods, and the one, the reaction of γ-chloropropyl triethoxysilane and sodium tetrasulfide obtains with distillation then after filtration in the presence of ethanol; The one, be that phase-transfer catalyst and nitrogen exist down with the Tetrabutyl amonium bromide, after γ-chloropropyl triethoxysilane and the aqueous sodium polysulfide reaction, isolate bottom water, obtain with distillation after filtration.In the preparation of Si-69, distillation is the important step in producing, and the installation of the type selecting of distillation plant, distillation auxiliary facility, the type of filler, reflux ratio etc. are very big to influences such as product inherence and external quality, product yield and economic benefits.Therefore existing Si-69 water distilling apparatus mostly is the simple distillation device greatly, and mainly contain following deficiency in actual production: (1) front-end volatiles amount is too many, cuts apart unintelligiblely with after cut, causes product yield low: the product colour after (2) distillation is rubescent or be deep yellow; (3) can cause portioned product to produce in the still-process and decompose, cause sulphur content total in the product index undesirable, precipitation or layering in product is stored, occur, influence the storage time.In addition, because Si-69 distinctive molecular structure and physical and chemical performance, except rubber industry, at present Si-69 in the special mechanical casting, to halloysite nanotubes (Halloysite nanotubes, HNTs) surface modification, contain fields such as the preparation of long carbon chain compound of S and Si and textile auxiliary agent be synthetic simultaneously and cause concern, and progressively be developed and applied, but above-mentioned industry is very high to the purity requirement of Si-69 product, and domestic currently available products content only is about 95% (GC) (amounting to), is difficult to satisfy the use needs of these industries.Given this, existing water distilling apparatus is transformed to improve product purity, productivity effect and product yield, important practical sense is arranged.
Summary of the invention
Technical problem to be solved in the utility model is: provide a kind of pair-[propyl-triethoxysilicane]-tetrasulfide water distilling apparatus, the product purity and the low problem of yield that exist in-[propyl-triethoxysilicane]-tetrasulfide distillation two in the prior art to solve.
For solving the problems of the technologies described above, the technical solution of the utility model is:
Two-[propyl-triethoxysilicane]-tetrasulfide water distilling apparatus, comprise still kettle, distillation tower, condenser and receiving tank that order is communicated with, described distillation tower comprises bottom column joint, middle part tower joint and upper column joint, is respectively equipped with bottom backflow pipe nipple and top backflow pipe nipple between described bottom column joint and described middle part tower joint, described middle part tower joint and the described upper column joint.
As a kind of improvement, be equipped with the backflow spray equipment in described top backflow pipe nipple and the bottom backflow pipe nipple, described backflow spray equipment is respectively equipped with the top return line and the bottom return line is communicated with the bottom of receiving tank.
As further improvement, be equipped with filler in described bottom column joint, middle part tower joint and the upper column joint.。
Owing to adopted technique scheme, the beneficial effects of the utility model are:
1, distillation tower of the present utility model comprises three towers joint, and between the tower joint backflow pipe nipple is set, and has cushioned the contact of liquid and gas in the still-process, reduces or has prevented the liquid flooding phenomenon.
2, the utility model adopts dual reflux to regulate gas-liquid two-phase material composition, can regulate reflux ratio according to the variation of product purity in the withdrawing can, by changing the implantation site that adds of withdrawing fluid, effectively improved distilling effect, improved the purity of distillage, product purity reaches more than 98% (GC), distillation residue have been reduced, product foreign matter content≤1% (GC) has enlarged the Application Areas of product, has also improved product yield simultaneously.
3, withdrawing can of the present utility model is provided with vacuum interface, can adopt decompression operation during distillation procedure, because of distillation temperature reduces, not only reduced energy consumption, and significantly reduced the decomposition of product Si-69, product colour is faint yellow to colourless, uses the product of the comparable existing simple distillation explained hereafter of Si-69 period of storage of the utility model production to prolong more than six months cost decreases about 5%.
4, the utility model is equipped with the backflow spray equipment in the backflow pipe nipple, after gas material enters the backflow pipe nipple, because gas, the mixing of liquid biphase and heat and mass have further been strengthened in the effect of liquid spraying, has improved the product separation effect.
Description of drawings
Below in conjunction with drawings and Examples the utility model is further specified.
Fig. 1 is the structural representation of the utility model embodiment.
Among the figure, 1. still kettle; 2. distillation tower; 21. bottom column joint; 22. middle part tower joint; 23. upper column joint; 24. bottom backflow pipe nipple; 25. top backflow pipe nipple; 3. condenser; 4. withdrawing can; 41. vacuum interface; 5. backflow spray equipment; 6. top return line; 7. bottom return line; 8. filler.
Embodiment
As shown in the figure, two-[propyl-triethoxysilicane]-tetrasulfide water distilling apparatus, comprise still kettle 1, distillation tower 2, condenser 3 and receiving tank 4 that order is communicated with, described receiving tank 4 is provided with vacuum interface 41, described distillation tower 1 comprises bottom column joint 21, middle part tower joint 22 and upper column joint 23, is respectively equipped with bottom backflow pipe nipple 24 and top backflow pipe nipple 25 between described bottom column joint 21 and middle part tower joint 22, middle part tower joint 22 and the upper column joint 23.Be equipped with backflow spray equipment 5 in described top backflow pipe nipple 24 and the bottom backflow pipe nipple 25, described backflow spray equipment 5 is respectively equipped with top return line 6 and bottom return line 7 is connected with the bottom of receiving tank 4, is equipped with filler 8 in described bottom column joint 21, middle part tower joint 22 and the upper column joint 23.
During the utility model work, distill under normal pressure earlier, steam the part low-boiling-point substance, its main component is low-sulfur silicon-containing compound, second alcohol and water, continues distillation then under reduced pressure, steams low-boiling-point substances such as disulphide, γ 2.After the content of Si-69 in the withdrawing can 4 reaches certain value, to open top return line 6, and regulate suitable reflux ratio, the liquid in the receiving tank 4 enters top backflow pipe nipple 25.In still-process, in the uphill process to upper column joint 23, the closer to upper column joint 23, the volatile components proportion is big more from bottom column joint 21 for steam; The closer to bottom column joint 21, difficult volatiles proportion is big more, therefore the liquid in the withdrawing can 4 is added fashionablely from top backflow pipe nipple 25, contains the vapor generation condensation of volatile components, and condensing droplet falls; Contact with the steam that continue to rise in the dropping process and heat exchange takes place, and under lower temperature, gasify once again, so the content of low boiling component will be more than the low boiling component in the condensing droplet in the steam.The process of such gasification-condensation is carried out repeatedly in middle part tower joint 22, finally obtains the very high Si-69 product of purity, and is regulating under the suitable reflux ratio, and it is stable that the content of Si-69 can keep.
Because what Si-69 adopted is batch distillation, along with distillatory carries out, the transformation by maximum decline will appear in product content.Under the constant prerequisite of operational condition, the quantity of steam of rising also slightly descends, and the Si-69 product content also has decline in the steam simultaneously.For guaranteeing Si-69 higher purity in the receiving tank 4, when descending, Si-69 content closes top return line 6 valves, open the valve of bottom return line 7, regulate suitable reflux ratio, liquid in the receiving tank 4 enters bottom backflow pipe nipple 24, liquid phase directly contacts with the gas phase that saves 21 from bottom column, carry out vapour-liquid phase mass transfer, the result is that the difficult volatiles in the gas phase partly changes liquid phase over to, volatile components in the liquid phase partly changes gas phase over to, the part vaporization of liquid phase and the partial condensation of vapour phase have promptly been realized simultaneously, save repeatedly vaporization-condensation of 23 through middle part tower joint 22 and upper column again, contain the higher steam of Si-69 purity and behind condenser 3, enter receiving tank 4, finally obtained the Si-69 product of the higher and stable content of purity by upper column joint 23.
Claims (3)
1. two-[propyl-triethoxysilicane]-tetrasulfide water distilling apparatus, comprise still kettle, distillation tower, condenser and receiving tank that order is communicated with, it is characterized in that: described distillation tower comprises bottom column joint, middle part tower joint and upper column joint, is respectively equipped with bottom backflow pipe nipple and top backflow pipe nipple between described bottom column joint and described middle part tower joint, described middle part tower joint and the described upper column joint.
2. as claimed in claim 1 pair-[propyl-triethoxysilicane]-tetrasulfide water distilling apparatus, it is characterized in that: be equipped with the backflow spray equipment in described top backflow pipe nipple and the bottom backflow pipe nipple, described backflow spray equipment is respectively equipped with the top return line and the bottom return line is communicated with the bottom of receiving tank.
3. as claimed in claim 1 pair-[propyl-triethoxysilicane]-tetrasulfide water distilling apparatus, it is characterized in that: be equipped with filler in described bottom column joint, middle part tower joint and the upper column joint.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010201539863U CN201722313U (en) | 2010-04-07 | 2010-04-07 | Double-propyltriethoxysilane four-sulfide distillation apparatus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010201539863U CN201722313U (en) | 2010-04-07 | 2010-04-07 | Double-propyltriethoxysilane four-sulfide distillation apparatus |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN201722313U true CN201722313U (en) | 2011-01-26 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010201539863U Expired - Fee Related CN201722313U (en) | 2010-04-07 | 2010-04-07 | Double-propyltriethoxysilane four-sulfide distillation apparatus |
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| Country | Link |
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| CN (1) | CN201722313U (en) |
Cited By (2)
| 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 |
| CN116212796A (en) * | 2023-03-29 | 2023-06-06 | 浙江润禾有机硅新材料有限公司 | Silicone oil production system |
-
2010
- 2010-04-07 CN CN2010201539863U patent/CN201722313U/en not_active Expired - Fee Related
Cited By (3)
| 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 |
| CN116212796A (en) * | 2023-03-29 | 2023-06-06 | 浙江润禾有机硅新材料有限公司 | Silicone oil production system |
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| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| ASS | Succession or assignment of patent right |
Owner name: QINGDAO RONGDA NEW MATERIALS RESEARCH INSTITUTE Free format text: FORMER OWNER: WEIFANG ZHONGSHI CHEMICAL CO., LTD. Effective date: 20120518 |
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| C41 | Transfer of patent application or patent right or utility model | ||
| COR | Change of bibliographic data |
Free format text: CORRECT: ADDRESS; FROM: 262737 WEIFANG, SHANDONG PROVINCE TO: 266612 QINGDAO, SHANDONG PROVINCE |
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| TR01 | Transfer of patent right |
Effective date of registration: 20120518 Address after: 266612 Shandong Province, Qingdao Laixi city and town resident Patentee after: Qingdao Rongda Institue of New Materials Address before: Binhai Economic Development Zone, Shandong city of Weifang province Dajiawa 262737 streets in Weifang Haihua Street South Lion Chemical Limited by Share Ltd Patentee before: Weifang Zhongshi Chemical Co., Ltd. |
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| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20110126 Termination date: 20130407 |