CN106085277A - A kind of preparation method of silicone sealant hydrophilic nano-silicon dioxide - Google Patents
A kind of preparation method of silicone sealant hydrophilic nano-silicon dioxide Download PDFInfo
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- CN106085277A CN106085277A CN201610597100.6A CN201610597100A CN106085277A CN 106085277 A CN106085277 A CN 106085277A CN 201610597100 A CN201610597100 A CN 201610597100A CN 106085277 A CN106085277 A CN 106085277A
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- Prior art keywords
- silicone sealant
- silicon dioxide
- nano
- hydrophilic nano
- preparation
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention discloses the preparation method of a kind of silicone sealant hydrophilic nano-silicon dioxide, relate to technical field of nano material, with waterglass and concentrated hydrochloric acid as raw material, prepare nano silicon, recycling hydrolytic polymaleic anhydride, tetrabutylammonium chloride, PEG400 and polyoxyethylene lauryl ether carry out chemical modification to it, preparing hydrophilic nano-silicon dioxide, granularity reaches 20 30nm.The made hydrophilic nano-silicon dioxide of the present invention is applied in silicone sealant, the hardening time of silicone sealant and water can not only be shortened, the caking property of silicone sealant, weatherability, vibration resistance and resistant of high or low temperature can also be strengthened, effectively expand the range of fluid sealant.
Description
Technical field:
The present invention relates to technical field of nano material, be specifically related to a kind of silicone sealant hydrophilic nano-silicon dioxide
Preparation method.
Background technology:
Silicone sealant is with polydimethylsiloxane as primary raw material, be aided with cross-linking agent, filler, plasticizer, coupling agent,
The paste that catalyst mixes under vacuum conditions, at room temperature by solidifying to form flexible silicon with the water in air
Rubber.Nano silicon, owing to belonging to ultrafine nanometer, therefore has much unique character, it is possible to be greatly improved material
Intensity, aging resistance, chemically-resistant and weatherability, but its hydrophilic is limited, after especially mixing with remaining raw material of silicone sealant
Hydrophilic is substantially reduced, impact and the solidification of water, it is therefore desirable to the structure of nano silicon is carried out chemical modification, to improve
Its hydrophilic.
Summary of the invention:
The technical problem to be solved is provide a kind of narrow particle size distribution and be conducive to improving silicone sealant
The preparation method of the silicone sealant hydrophilic nano-silicon dioxide of weatherability, vibration resistance and resistant of high or low temperature.
The technical problem to be solved uses following technical scheme to realize:
The preparation method of a kind of silicone sealant hydrophilic nano-silicon dioxide, comprises the steps:
(1) stirring under in the water glass solution of mass concentration 40% drip concentrated hydrochloric acid, control solution ph at 5-6, then
Microwave treatment 10min under microwave frequency 2450MHz, power 700W, then naturally cools to 50-60 DEG C, continues after insulation 3h
Microwave treatment 5min, gained mixed solution stands 8h at 0-5 DEG C, filters, and filtering residue is washed three times, finally at 100-110 DEG C
It is dried 5h, obtains intermediate compound I；
(2) by intermediate compound I grind into powder, add hydrolytic polymaleic anhydride and tetrabutylammonium chloride, grind 1h backward
Mixed-powder adds isopropanol, after being sufficiently mixed, stands 30min, then microwave under microwave frequency 2450MHz, power 700W
Process 10min, obtain intermediate II；
(3) adding PEG400 and polyoxyethylene lauryl ether in intermediate II, mix homogeneously post-heating is to backflow
State insulation 30min, insulation is lowered the temperature with 5 DEG C/min after terminating under ice-water bath, until temperature is down to-5 DEG C, then protects at-5 DEG C
Temperature 3h, then filters, and gained filtering residue is dried 3h at 80-90 DEG C, finally calcines 2h at 550-600 DEG C.
Described waterglass, hydrolytic polymaleic anhydride, tetrabutylammonium chloride, isopropanol, PEG400 and lauryl alcohol polyoxy
The amount ratio of vinyl Ether is 1:0.15:0.02:3:0.05:0.03.
The invention has the beneficial effects as follows: the present invention, with waterglass and concentrated hydrochloric acid as raw material, prepares nano silicon, then profit
With hydrolytic polymaleic anhydride, tetrabutylammonium chloride, PEG400 and polyoxyethylene lauryl ether, it is carried out chemical modification,
Preparing hydrophilic nano-silicon dioxide, granularity reaches 20-30nm；Made hydrophilic nano-silicon dioxide is applied to silicone seal
In glue, the hardening time of silicone sealant and water can not only be shortened, moreover it is possible to strengthen the caking property of silicone sealant, weatherability, resist
Shaking property and resistant of high or low temperature, effectively expand the range of fluid sealant.
Detailed description of the invention:
For the technological means making the present invention realize, creation characteristic, reach purpose and be easy to understand with effect, below knot
Close specific embodiment, the present invention is expanded on further.
Embodiment 1
(1) under stirring, in the water glass solution (adding water formulated with 10g waterglass) of mass concentration 40%, dropping is dense
Hydrochloric acid, controls solution ph at 5-6, and microwave treatment 10min under microwave frequency 2450MHz, power 700W is the coldest
But to 50-60 DEG C, continuing microwave treatment 5min after insulation 3h, gained mixed solution stands 8h at 0-5 DEG C, filters, filtering residue water
Wash three times, at 100-110 DEG C, be finally dried 5h, obtain intermediate compound I；
(2) by intermediate compound I grind into powder, add 1.5g hydrolytic polymaleic anhydride and 0.2g tetrabutylammonium chloride, grind
In mixed-powder, add 30g isopropanol after mill 1h, stand 30min after being sufficiently mixed, then in microwave frequency 2450MHz, merit
Microwave treatment 10min under rate 700W, obtains intermediate II；
(3) in intermediate II, add 0.5g PEG400 and 0.3g polyoxyethylene lauryl ether, add after mix homogeneously
Heat to reflux state is incubated 30min, and insulation is lowered the temperature with 5 DEG C/min after terminating under ice-water bath, until temperature is down to-5 DEG C, then
Being incubated 3h at-5 DEG C, then filter, gained filtering residue is dried 3h at 80-90 DEG C, finally calcines 2h at 550-600 DEG C i.e.
Can.
The ultimate principle of the present invention and principal character and advantages of the present invention have more than been shown and described.The technology of the industry
Personnel, it should be appreciated that the present invention is not restricted to the described embodiments, simply illustrating this described in above-described embodiment and description
The principle of invention, without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications, and these become
Change and improvement both falls within scope of the claimed invention.Claimed scope by appending claims and
Equivalent defines.
Claims (2)
1. the preparation method of a silicone sealant hydrophilic nano-silicon dioxide, it is characterised in that comprise the steps:
(1) dripping concentrated hydrochloric acid under stirring in the water glass solution of mass concentration 40%, control solution ph is at 5-6, then at micro-
Microwave treatment 10min under wave frequency 2450MHz, power 700W, then naturally cools to 50-60 DEG C, continues microwave after insulation 3h
Processing 5min, gained mixed solution stands 8h at 0-5 DEG C, filters, and filtering residue is washed three times, is finally dried at 100-110 DEG C
5h, obtains intermediate compound I；
(2) by intermediate compound I grind into powder, hydrolytic polymaleic anhydride and tetrabutylammonium chloride are added, to mixing after grinding 1h
Powder adds isopropanol, after being sufficiently mixed, stands 30min, then microwave treatment under microwave frequency 2450MHz, power 700W
10min, obtains intermediate II；
(3) adding PEG400 and polyoxyethylene lauryl ether in intermediate II, mix homogeneously post-heating is to reflux state
Insulation 30min, insulation is lowered the temperature with 5 DEG C/min after terminating under ice-water bath, until temperature is down to-5 DEG C, then is incubated at-5 DEG C
3h, then filters, and gained filtering residue is dried 3h at 80-90 DEG C, finally calcines 2h at 550-600 DEG C.
The preparation method of silicone sealant hydrophilic nano-silicon dioxide the most according to claim 1, it is characterised in that:
Described waterglass, hydrolytic polymaleic anhydride, tetrabutylammonium chloride, isopropanol, PEG400 and polyoxyethylene lauryl ether
Amount ratio is 1:0.15:0.02:3:0.05:0.03.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610597100.6A CN106085277A (en) | 2016-07-26 | 2016-07-26 | A kind of preparation method of silicone sealant hydrophilic nano-silicon dioxide |
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| CN201610597100.6A CN106085277A (en) | 2016-07-26 | 2016-07-26 | A kind of preparation method of silicone sealant hydrophilic nano-silicon dioxide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106751859A (en) * | 2016-12-20 | 2017-05-31 | 湖北环宇化工有限公司 | A kind of method that dealcoholized silicone rubber is prepared with microwave treatment hydrophilic white carbon |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105255220A (en) * | 2015-10-19 | 2016-01-20 | 佛山科学技术学院 | Nano SiO2 surface modification method |
-
2016
- 2016-07-26 CN CN201610597100.6A patent/CN106085277A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105255220A (en) * | 2015-10-19 | 2016-01-20 | 佛山科学技术学院 | Nano SiO2 surface modification method |
Non-Patent Citations (6)
| Title |
|---|
| 李广宇等: "《胶黏剂原材料手册》", 31 August 2004 * |
| 潘卫三: "《工业药剂学》", 31 August 2015 * |
| 焦学瞬: "《表面活性剂实用新技术》", 31 May 1996 * |
| 符韵林等: "《用二氧化硅改良木材表面性能的研究》", 31 October 2011 * |
| 解一军等: "《溶剂应用手册》", 31 July 2009 * |
| 郭宇等: "化学沉淀法制备纳米二氧化硅", 《辽宁化工》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106751859A (en) * | 2016-12-20 | 2017-05-31 | 湖北环宇化工有限公司 | A kind of method that dealcoholized silicone rubber is prepared with microwave treatment hydrophilic white carbon |
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Application publication date: 20161109 |