CN105503936A - Method for decreasing chlorine ion content in polymethyl triethoxy silane product - Google Patents
Method for decreasing chlorine ion content in polymethyl triethoxy silane product Download PDFInfo
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- CN105503936A CN105503936A CN201510970456.5A CN201510970456A CN105503936A CN 105503936 A CN105503936 A CN 105503936A CN 201510970456 A CN201510970456 A CN 201510970456A CN 105503936 A CN105503936 A CN 105503936A
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- reaction
- sherwood oil
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- ion content
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- 238000000034 method Methods 0.000 title claims abstract description 37
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 title claims abstract description 17
- 230000003247 decreasing effect Effects 0.000 title abstract 3
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 title abstract 3
- 238000006243 chemical reaction Methods 0.000 claims abstract description 47
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 34
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 claims abstract description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 17
- 238000004821 distillation Methods 0.000 claims abstract description 14
- 230000035484 reaction time Effects 0.000 claims abstract description 6
- 241000370738 Chlorion Species 0.000 claims description 20
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 20
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 17
- 239000000460 chlorine Substances 0.000 abstract description 6
- 229910052801 chlorine Inorganic materials 0.000 abstract description 6
- -1 chlorine ions Chemical class 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 abstract 10
- 239000003208 petroleum Substances 0.000 abstract 5
- 239000012295 chemical reaction liquid Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 32
- 238000011084 recovery Methods 0.000 description 9
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 7
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 239000007789 gas Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010792 warming 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
-
- 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
- C07F7/188—Preparation; Treatments not provided for in C07F7/20 by reactions involving the formation of Si-O linkages
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
Abstract
The invention discloses a method for decreasing the chlorine ion content in a polymethyl triethoxy silane product. The method comprises the following steps that an appropriate amount of methyl trichloro silicane is put into a reaction kettle through a feeding pump, the reaction temperature in the reaction kettle is controlled to range from 60 DEG C to 90 DEG C, an appropriate amount of absolute ethyl alcohol is dropwise added into the reaction kettle through an elevated tank, an appropriate amount of nitrogen is fed into the reaction kettle simultaneously to speed up the reaction, an appropriate amount of petroleum ether is added, the reaction time is controlled to range from 3 h to 5 h, and chlorine ions produced in the reaction are wrapped with the petroleum ether; after the reaction is completed, distillation treatment is conducted on reaction liquid to recycle the petroleum ether, and the polymethyl triethoxy silane product is obtained finally. According to the method, the corresponding amount of the petroleum ether is added, the chlorine ions replaced with oxethyl are wrapped with the petroleum ether, the free activity of the chlorine ions is reduced, the content of the chlorine ions in the product is effectively decreased, the chlorine ions are controlled to 10 PPM or below, the product quality is improved, and the application field of the product is enlarged.
Description
Technical field
The present invention relates to a kind of method reducing chloride ion content in poly-Union carbide A-162 product.
Background technology
When synthesizing poly-Union carbide A-162, in reactor, squeezing into the monomethyl trichlorosilane measured, be warmed up to 60 ~ 90 degree, in still, dripping dehydrated alcohol from dehydrated alcohol header tank, passing into nitrogen bubble and carry out back flow reaction.Monomethyl trichlorosilane and dehydrated alcohol react and generate poly-Union carbide A-162 and hydrogenchloride, and the object of logical nitrogen is the discharge driving by-product micromolecular compound hydrogen chloride tail gas.In temperature rising reflux reaction process, the air-flow of rising enters condenser by a straight blank pipe, and phlegma is back to reactor, and solidifying gas chlorination hydrogen removes tail gas absorption, and reaction terminates, and reaction solution remaining in still is exactly poly-Union carbide A-162 product.Owing to generating a large amount of hydrogen chloride gas in reaction process, although urge and catch hydrogenchloride by means of nitrogen bubble, part must be also had residual.Because material can not adiabatic drying, air-flow also can the moisture absorption in condensation process, and make the moisture of product tape trace, cause product free chlorine ion content higher, the free chlorine of common product is at more than 50PPM.Chlorion is higher, and the Application Areas of product is subject to certain restrictions, and has many high-end occasions not use.
Summary of the invention
The present invention is directed to the deficiencies in the prior art part, there is provided that a kind of method is simple, labour intensity is low, improve product quality obviously, the reduction of continuous operation can gather the method for chloride ion content in Union carbide A-162 product, the method is prepared in the process that monomethyl trichlorosilane and dehydrated alcohol react, add the sherwood oil of respective amount, wrapped up by sherwood oil by the chlorion that oxyethyl group replaces, reduce its free activity.After completion of the reaction, first Distillation recovery sherwood oil, in still-process, chlorion or hydrogenchloride are also easily taken out of, and the sherwood oil then reusable edible of Distillation recovery, then normally goes out product.Whole conversion unit and process do not do large change, just increase a kind of raw material sherwood oil when feeding intake, and reaction terminates this part sherwood oil of rear first Distillation recovery and feeds intake for next batch again.Facts have proved, by adding this method of sherwood oil, significantly reducing the content of chlorion in product, make chlorion control, at below 10PPM, to improve product quality, expand the Application Areas of product.
In order to solve the problems of the technologies described above, adopt following technical scheme:
A kind of method reducing chloride ion content in poly-Union carbide A-162 product, comprise the following steps: first by fresh feed pump, appropriate monomethyl trichlorosilane is put in reactor, the temperature of reaction controlled in reactor is 60 ~ 90 DEG C, header tank is utilized to drip appropriate dehydrated alcohol in still, the mol ratio of monomethyl trichlorosilane and dehydrated alcohol is 1: (2 ~ 4), meanwhile in reactor, pass into appropriate nitrogen, back flow reaction is carried out by nitrogen bubble, accelerate to carry out corresponsively, and add appropriate sherwood oil, the mol ratio of monomethyl trichlorosilane and sherwood oil is 1: (3 ~ 6), the control reaction times is 3 ~ 5h, the chlorion that reaction produces is wrapped up by sherwood oil, after the completion of reaction, reaction solution is carried out distillation process, reclaim sherwood oil, finally obtain poly-Union carbide A-162 product.
After optimization, the mol ratio of monomethyl trichlorosilane and dehydrated alcohol is 1: (2.5 ~ 3.5).
After optimization, the mol ratio of monomethyl trichlorosilane and sherwood oil is 1: (4 ~ 5).
Further, sherwood oil is the sherwood oil of the sherwood oil of 30 ~ 60#, the sherwood oil of 60 ~ 90# or 90 ~ 120#.
Further, nitrogen passes into the flow velocity in reactor is 180mL/min.
Owing to adopting technique scheme, there is following beneficial effect:
The present invention is a kind of method reducing chloride ion content in poly-Union carbide A-162 product, the method method is simple, labour intensity is low, improve product quality obviously, can continuous operation.The method is prepared in the process that monomethyl trichlorosilane and dehydrated alcohol react, and adds the sherwood oil of respective amount, is wrapped up by the chlorion that oxyethyl group replaces by sherwood oil, reduce its free activity.After completion of the reaction, first Distillation recovery sherwood oil, in still-process, chlorion or hydrogenchloride are also easily taken out of, and the sherwood oil then reusable edible of Distillation recovery, then normally goes out product.Whole conversion unit and process do not do large change, just increase a kind of raw material sherwood oil when feeding intake, and reaction terminates this part sherwood oil of rear first Distillation recovery and feeds intake for next batch again.Facts have proved, by adding this method of sherwood oil, significantly reducing the content of chlorion in product, make chlorion control, at below 10PPM, to improve product quality, expand the Application Areas of product.
Embodiment
A kind of method reducing chloride ion content in poly-Union carbide A-162 product, monomethyl trichlorosilane and dehydrated alcohol is selected to be reaction raw materials, back flow reaction is carried out by nitrogen bubble, add the sherwood oil of respective amount, wrapped up by sherwood oil by the chlorion that oxyethyl group replaces, reduce its free activity, significantly reduce the content of chlorion in product, make chlorion control, at below 10PPM, to improve product quality, the chemical equation that relates generally to of its reaction is:
Concrete reaction process is as follows: first put in reactor by fresh feed pump by appropriate monomethyl trichlorosilane, the temperature of reaction controlled in reactor is 60 ~ 90 DEG C, header tank is utilized to drip appropriate dehydrated alcohol in still, the mol ratio of monomethyl trichlorosilane and dehydrated alcohol is 1: (2 ~ 4), the preferred molar ratio of monomethyl trichlorosilane and dehydrated alcohol is 1: (2.5 ~ 3.5), meanwhile in reactor, pass into appropriate nitrogen, the nitrogen flow velocity passed in reactor is 180mL/min, back flow reaction is carried out by nitrogen bubble, accelerate to carry out corresponsively, and add appropriate sherwood oil, sherwood oil is the sherwood oil of 30 ~ 60#, the sherwood oil of 60 ~ 90# or the sherwood oil of 90 ~ 120#, the mol ratio of monomethyl trichlorosilane and sherwood oil is 1: (3 ~ 6), the preferred molar ratio of monomethyl trichlorosilane and sherwood oil is 1: (4 ~ 5), the control reaction times is 3 ~ 5h, the chlorion that reaction produces is wrapped up by sherwood oil, after the completion of reaction, reaction solution is carried out distillation process, reclaim sherwood oil, finally obtain poly-Union carbide A-162 product.
The method is prepared in the process that monomethyl trichlorosilane and dehydrated alcohol react, and adds the sherwood oil of respective amount, is wrapped up by the chlorion that oxyethyl group replaces by sherwood oil, reduce its free activity.After completion of the reaction, first Distillation recovery sherwood oil, in still-process, chlorion or hydrogenchloride are also easily taken out of, and the sherwood oil then reusable edible of Distillation recovery, then normally goes out product.Whole conversion unit and process do not do large change, just increase a kind of raw material sherwood oil when feeding intake, and reaction terminates this part sherwood oil of rear first Distillation recovery and feeds intake for next batch again.Facts have proved, by adding this method of sherwood oil, significantly reducing the content of chlorion in product, make chlorion control, at below 10PPM, to improve product quality, expand the Application Areas of product.
Below in conjunction with embodiment, a kind of method reducing chloride ion content in poly-Union carbide A-162 product is described in further detail:
Embodiment 1
In the reaction of 1L, disposablely add monomethyl trichlorosilane 250g (1mol), start to stir, be warming up to 60 DEG C, in still, dehydrated alcohol 115g (2.5mol) is dripped with header tank, meanwhile in reactor, pass into appropriate nitrogen, the nitrogen flow velocity passed in reactor is 180mL/min, back flow reaction is carried out by nitrogen bubble, accelerate to carry out corresponsively, and add the sherwood oil 250g (3mol) of 30 ~ 60#, the control reaction times is 3 ~ 5h, the chlorion that reaction produces is wrapped up by described sherwood oil, after the completion of reaction, reaction solution is carried out distillation process, reclaim sherwood oil 220.5g, finally obtain poly-Union carbide A-162 product 95.5g, productive rate is 83.8%, in poly-Union carbide A-162, chloride ion content is 9.8PPM.
Embodiment 2 ~ 9
Adopt with the identical synthesis step of embodiment 1, concrete formula refers to table 1, and concrete technology condition and product yield refer to table 2.
Table 1
Table 2
| Project | Temperature of reaction (DEG C) | Reaction times (h) | Chloride ion content (PPM) | Yield |
| Embodiment 2 | 65 | 3 | 8.8 | 87.1％ |
| Embodiment 3 | 70 | 3 | 9.6 | 87.3％ |
| Embodiment 4 | 75 | 4 | 9.4 | 90.3％ |
| Embodiment 5 | 80 | 4 | 8.9 | 90.1％ |
| Embodiment 6 | 85 | 4 | 8.7 | 90.6％ |
| Embodiment 7 | 90 | 5 | 9.6 | 93.9％ |
| Embodiment 8 | 75 | 5 | 9.8 | 93.3％ |
| Embodiment 9 | 85 | 5 | 9.9 | 93.3％ |
These are only specific embodiments of the invention, but technical characteristic of the present invention is not limited thereto.Any based on the present invention, for solving substantially identical technical problem, realize substantially identical technique effect, done ground simple change, equivalent replacement or modification etc., be all covered by among protection scope of the present invention.
Claims (5)
1. one kind is reduced the method for chloride ion content in poly-Union carbide A-162 product, it is characterized in that comprising the following steps: first by fresh feed pump, appropriate monomethyl trichlorosilane is put in reactor, the temperature of reaction controlled in reactor is 60 ~ 90 DEG C, header tank is utilized to drip appropriate dehydrated alcohol in still, the mol ratio of described monomethyl trichlorosilane and described dehydrated alcohol is 1: (2 ~ 4), meanwhile in reactor, pass into appropriate nitrogen, back flow reaction is carried out by described nitrogen bubble, accelerate to carry out corresponsively, and add appropriate sherwood oil, the mol ratio of described monomethyl trichlorosilane and described sherwood oil is 1: (3 ~ 6), the control reaction times is 3 ~ 5h, the chlorion that reaction produces is wrapped up by described sherwood oil, after the completion of reaction, reaction solution is carried out distillation process, reclaim described sherwood oil, finally obtain poly-Union carbide A-162 product.
2. a kind of method reducing chloride ion content in poly-Union carbide A-162 product according to claim 1, is characterized in that: the mol ratio of described monomethyl trichlorosilane and described dehydrated alcohol is 1: (2.5 ~ 3.5).
3. a kind of method reducing chloride ion content in poly-Union carbide A-162 product according to claim 1, is characterized in that: the mol ratio of described monomethyl trichlorosilane and described sherwood oil is 1: (4 ~ 5).
4. a kind of method reducing chloride ion content in poly-Union carbide A-162 product according to claim 1, is characterized in that: described sherwood oil is the sherwood oil of the sherwood oil of 30 ~ 60#, the sherwood oil of 60 ~ 90# or 90 ~ 120#.
5. a kind of method reducing chloride ion content in poly-Union carbide A-162 product according to claim 1, is characterized in that: the described nitrogen flow velocity passed in reactor is 180mL/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510970456.5A CN105503936A (en) | 2015-12-21 | 2015-12-21 | Method for decreasing chlorine ion content in polymethyl triethoxy silane product |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510970456.5A CN105503936A (en) | 2015-12-21 | 2015-12-21 | Method for decreasing chlorine ion content in polymethyl triethoxy silane product |
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| Publication Number | Publication Date |
|---|---|
| CN105503936A true CN105503936A (en) | 2016-04-20 |
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| CN201510970456.5A Pending CN105503936A (en) | 2015-12-21 | 2015-12-21 | Method for decreasing chlorine ion content in polymethyl triethoxy silane product |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102372733A (en) * | 2011-11-30 | 2012-03-14 | 江苏创基新材料有限公司 | Continuous preparation method for methyl trialkoxysilane |
| CN104610335A (en) * | 2015-01-27 | 2015-05-13 | 荆州市江汉精细化工有限公司 | Industrial continuous preparation method of triethoxy hydrosilane |
-
2015
- 2015-12-21 CN CN201510970456.5A patent/CN105503936A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102372733A (en) * | 2011-11-30 | 2012-03-14 | 江苏创基新材料有限公司 | Continuous preparation method for methyl trialkoxysilane |
| CN104610335A (en) * | 2015-01-27 | 2015-05-13 | 荆州市江汉精细化工有限公司 | Industrial continuous preparation method of triethoxy hydrosilane |
Non-Patent Citations (1)
| Title |
|---|
| 许健 等: ""甲基三乙氧基硅烷的制备工艺研究"", 《杭州师范大学学报（自然科学版）》 * |
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