CN108530679A - A kind of in-situ modified method for preparing nano silicon dioxide composite antioxidant - Google Patents
A kind of in-situ modified method for preparing nano silicon dioxide composite antioxidant Download PDFInfo
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- CN108530679A CN108530679A CN201810381302.6A CN201810381302A CN108530679A CN 108530679 A CN108530679 A CN 108530679A CN 201810381302 A CN201810381302 A CN 201810381302A CN 108530679 A CN108530679 A CN 108530679A
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- antioxidant
- silicon dioxide
- nano silicon
- dioxide composite
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses a kind of in-situ modified methods for preparing nano silicon dioxide composite antioxidant, on the one hand on the other hand the temperature in use for improving antioxidant 1330 solves nano silicon dioxide itself bad dispersibility, twice dispersing modified technique complexity, the big and heavy-polluted drawback of energy consumption.On the basis of sol-gel technique, the excellent nano silicon dioxide composite antioxidant of the in-situ modified preparation uniform particle sizes of the technologies such as antioxidant itself functional group, dosage, addition temperature, addition time, reaction condition, exterior appearance is utilized.This preparation and method of modifying technique are advanced, informative data is accurate, product is white powder graininess, 80 120nm of particle diameter, can the multiple fields application such as anti-oxidant, activeness and quietness and industrial coating in macromolecule, be the preparation method of very ideal nano silicon dioxide composite antioxidant.
Description
Technical field
The present invention relates to a kind of in-situ modified methods for preparing nano silicon dioxide composite antioxidant, belong to inorganic nano material
Preparation and application technical field.
Background technology
Antioxidant 1330 belongs to high molecular weight polyhydric Hinered phenols antioxidant, has do not pollute, is not colored, volatility is low etc.
Feature is the excellent antioxidant of high density polyethylene (HDPE), polypropylene and rubber, be chiefly used in polyvinyl chloride, polyamide, ABS resin and
The plastic products such as polyester.But its fusing point is 240 DEG C or so, easily decomposes in process, influences the product of process and product
Matter.
Nano silicon dioxide has good thermal stability, thickening property, reinforcing etc..It is widely used in rubber, engineering plastic
It is the ultra tiny inorganic green wood of extremely important high-tech in the composite modifications such as material, biomedicine, ceramics, building materials, resin base
One of material.But because nano silicon dioxide grain size it is smaller, surface-active is higher, production and application process in easily generate it is soft,
Hard aggregation causes application performance to reduce.
Invention content
The present invention is pyrolytic and during preparing nano silicon dioxide during solving current 1330 use of antioxidant
The technical issues of existing hard agglomeration phenomenon and complex process, provide that a kind of in-situ modified to prepare nano silicon dioxide compound
The method of antioxidant.
Realization that the present invention adopts the following technical solutions：One kind is in-situ modified to prepare nano silicon dioxide composite antioxidant
Method, the chemical substance material used is：Ethyl orthosilicate, the ammonium hydroxide for calculating a concentration of 25% based on mass fraction, anhydrous second
Alcohol, acetone, antioxidant 1330, deionized water, the liquid chemical substance material utilization amount are calculated with volume parts；Wherein, resist
The basic chemical property of oxygen agent 1330 is as follows：
Chemical name：1,3,5- trimethyls -2,4,6- three (3,5- di-t-butyl -4- hydroxyls benzyl) benzene
Molecular formula：C54H78O3
Molecular weight：775.2
Molecular structural formula：
Preparation method is as follows：
(1) selected each chemical substance material
(2) in-situ modified to prepare nano silicon dioxide composite antioxidant
1. preparing solution
49 ~ 51 parts of absolute ethyl alcohols are measured, are placed in beaker for use；It measures 24 ~ 36 parts of ammonium hydroxide and is placed in the conical flask with rubber stopper
In it is for use；5.0-5.2 parts of ethyl orthosilicate and 49-51 parts of absolute ethyl alcohol are measured, is placed in beaker and mixes, stirred with glass bar
Mixing keeps it for use after mixing；It measures antioxidant 1330 to be dissolved in 145-150 parts of acetone, stirs evenly and be prepared into third
Quality-volume ratio of ketone solution, antioxidant 1330 and acetone is 8 ~ 10：29~30mg/ml；It is placed in until completely dissolved with glass
It is for use in the conical flask of glass plug；
2. in-situ modified prepare nano silicon dioxide composite antioxidant process
Absolute ethyl alcohol and ammonia spirit are placed in three-necked flask, are subsequently placed in magnetic agitation heating mantle, turn on agitator is opened
Heating is opened, sets agitator speed as 200r/min, warm temperature is set as 65 DEG C, configures condensation reflux unit；In temperature raising period
Between when temperature reaches 45 DEG C, with the speed of 0.75 part/min will teos solution be added three-necked flask in；Condensing reflux
After reacting 1h, acetone soln is added drop-wise in three-necked flask with the speed of 0.25 part/min；Condensing reflux reacts 6h；
3. ultrasonic water bath dispersion reaction
Three-necked flask 2. after reaction, is placed in ultrasonic water bath pond that the reaction was continued by step, and bath temperature is 60 DEG C, supersonic frequency
Rate is 80KHz, power 90W, reaction time 2h；
4. washing filters
By step, 3. reaction mixture is placed in beaker, and 100-150 parts of absolute ethyl alcohol is added, and 3min is stirred, at cleaning solution；It will washing
Liquid filters to obtain filter cake, and filter cake is placed in 200-250 parts of absolute ethyl alcohols, cleaning solution is stirred into, and filters；It so carries out 5 times, obtains
To filter cake；
Filter cake is added in 200 parts of deionized waters, agitator treating 5min, at cleaning solution；Filtering and washing to filtrate is in neutrality, and obtains
Product cake；
5. drying is ground up, sieved
By step, 4. products therefrom filter cake is placed in vacuum drying chamber dry, 60 DEG C, vacuum degree 0.1MPa of drying temperature, when dry
Between 2h；
Powder after drying agate mortar, pestle are ground, is then sieved with 400 mesh screens, obtains nanometer titanium dioxide
Silicon composite antioxidant product.
The pattern of the nano silicon dioxide composite antioxidant of preparation, color and luster, ingredient, Chemical Physics performance are detected,
Analysis, characterization：
Morphology analysis is carried out to nano silicon dioxide composite antioxidant with JSM-6700F types field emission scanning electron microscope；
Thermal stability analysis is carried out to product with TGA4000 types thermogravimetric analyzer；
Conclusion：Nano silicon dioxide composite antioxidant made from the application is white powder particle, particle diameter 80-120nm, shape
Looks are regular, uniform particle sizes, well dispersed, Chemical Physics performance stabilization.
Nano silicon dioxide is stored in the glass container of amber transparent, closed to be protected from light storage, waterproof, sun-proof, acid-proof
Alkali salt corrodes, 25 DEG C of storage temperature, relative humidity≤10%.
Beneficial effects of the present invention：
The present invention has significantly advance compared with prior art, is for easily high temperature divides during 1330 use of antioxidant
The drawbacks of solution, nano silicon dioxide dispersibility is poor, aggregate is more, twice dispersing modified technique complexity, consuming energy, in original
On the basis of having sol-gel technique, changed in situ using technologies such as amount of modifier, addition time, addition temperature, reaction conditions
Property prepares that exterior appearance is excellent, nano silicon dioxide composite antioxidants of uniform particle sizes.This preparation and method of modifying technique it is advanced,
Informative data is accurate, and product is white powder graininess, and particle diameter 80-120nm can enhance in macromolecule antioxygen, industry applies
The multiple fields applications such as material, are the preparation methods of very ideal nano silicon dioxide composite antioxidant.
Further, step（1）The chemical substance material that uses of preparation to be carried out selected, and carry out quality purity, dense
Degree control：Ethyl orthosilicate purity is 99.9%, absolute ethyl alcohol purity 99.9%；Acetone purity 99.9%；1330 purity of antioxidant
99.9%；Deionized water purity 99.9%.
Further, 2. middle first condensing reflux reacts 1h to step, then acetone soln condensing reflux reaction 6h is added dropwise；Positive silicic acid
Ethyl ester solution rate of addition is 0.75 part/min, and acetone soln rate of addition is 0.25 part/min.
Further, step 4. in first washed, filter with absolute ethyl alcohol, then be washed with deionized, filter to filtrate and be in
It is neutral.
Nanometer two can effectively be ensured using the raw material of above-mentioned purity, material dropping time and speed, washing suction filtration number
The quality of silica composite antioxidant is more preferable.
Description of the drawings
Fig. 1 prepares nano silicon dioxide composite antioxidant state diagram to be in-situ modified.
Fig. 2 prepares nano silicon dioxide composite antioxidant ultrasound state diagram to be in-situ modified.
Fig. 3 is nano silicon dioxide composite antioxidant microscopic appearance figure.
Fig. 4 is nano silicon dioxide composite antioxidant hot weightless picture.
1- magnetic agitations heat block set, 2- three-necked flasks, 3- addition funnels, 4- liquid feeding control valves, 5- condensation reflux devices, 6-
Temperature inductor, 7- temperature inductor fixed frames, 8- is in-situ modified to prepare nano silicon dioxide composite antioxidant mixed liquor, and 9- adds
Liquid funnel fixing bracket, 10- condensation reflux device fixed frames, 11- magnetic agitation rotors, 12- the first temperature control knobs, 13- rotating speed controls
Button processed, 14- ultrasonic wave transmitting modules, 15- numerical control ultrasonic cleaner water-bath seats, 16- purified liquid waters, 17- power control knobs,
18- second temperature control knobs.
Specific implementation mode
A kind of in-situ modified method for preparing nano silicon dioxide composite antioxidant of embodiment 1, the chemicals material used
Material is：Ethyl orthosilicate, the ammonium hydroxide for calculating a concentration of 25% based on mass fraction, absolute ethyl alcohol, acetone, antioxidant 1330, deionization
Water.
Preparation method is as follows：
(1) selected each chemical substance material
(2) in-situ modified to prepare nano silicon dioxide composite antioxidant
1. preparing solution
51ml absolute ethyl alcohols are measured, are placed in beaker for use；29ml ammonium hydroxide is measured to be placed in the conical flask with rubber stopper for use；
5ml ethyl orthosilicates and 50ml absolute ethyl alcohols are measured, is placed in beaker and mixes, so that it is waited for after mixing with glass bar stirring
With；It measures 45mg antioxidant 1330 to be dissolved in the acetone of 150ml, stirs evenly and be prepared into acetone soln, until completely dissolved
It is placed in the conical flask with glass stopper for use.
2. in-situ modified prepare nano silicon dioxide composite antioxidant process
Absolute ethyl alcohol and ammonia spirit are placed in three-necked flask, are subsequently placed in magnetic agitation heating mantle, turn on agitator is opened
Heating is opened, sets agitator speed as 200r/min, warm temperature is set as 65 DEG C, configures condensation reflux unit.In temperature raising period
Between when temperature reaches 45 DEG C, with the speed of 0.75ml/min will teos solution be added three-necked flask in；Condensing reflux
After reacting 1h, acetone soln is added drop-wise in three-necked flask with the speed of 0.25ml/min；Condensing reflux reacts 6h.
3. ultrasonic water bath dispersion reaction
Three-necked flask 2. after reaction, is placed in ultrasonic water bath pond that the reaction was continued by step, and bath temperature is 60 DEG C, supersonic frequency
Rate is 80KHz, power 90W, reaction time 2h.
4. washing filters
By step, 3. reaction mixture is placed in beaker, and absolute ethyl alcohol 150ml is added, and 3min is stirred, at cleaning solution；Cleaning solution is taken out
Filter obtains filter cake, and filter cake is placed in 200ml absolute ethyl alcohols, cleaning solution is stirred into, and filters；It so carries out 5 times, obtains filter cake；
Filter cake is added in 200ml deionized waters, agitator treating 5min, at cleaning solution；Filtering and washing to filtrate is in neutrality, and obtains
Product cake.
5. drying is ground up, sieved
Product cake is placed in vacuum drying chamber to dry, 60 DEG C, vacuum degree 0.1MPa, drying time 2h of drying temperature；
Powder after drying agate mortar, pestle are ground, is then sieved with 400 mesh screens, obtains nanometer titanium dioxide
Silicon composite antioxidant product.
Below in conjunction with attached drawing, the present invention will be further described：
Shown in Fig. 1, nano silicon dioxide composite antioxidant state diagram is prepared to be in-situ modified, each portion position will correctly be matched according to quantity
Than sequentially operating.
The magnitude for preparing the chemical substance used is determined by preset range, is measurement unit with gram, milliliter.
Three-necked flask 2 is placed in magnetic agitation heating mantle 1, and the heating temperature of magnetic agitation heating mantle 1 is by the first temperature control
Button 12 processed controls；Addition funnel 3, condensation reflux device 5, temperature inductor are set gradually from left to right on the top of three-necked flask 2
6；3 lower part of addition funnel is equipped with liquid feeding control valve 4, and is fixed by addition funnel fixed frame 9；Condensation reflux device 5 is by condensing reflux
Device control cage 10 is fixed；Temperature inductor 6 is fixed by inductor fixed mount 7；It is in-situ modified preparation nanometer two in three-necked flask 2
Silica composite antioxidant mixed liquor 8；Magnetic agitation rotor 11 is arranged at 2 bottom of three-necked flask；11 rotating speed of magnetic agitation rotor is by turning
Fast control knob 13 controls.
Fig. 2 prepares nano silicon dioxide composite antioxidant ultrasound bath figure to be in-situ modified, and each portion position is correct, presses
Amount proportioning, sequentially operates.
Three-necked flask 2 is placed on numerical control ultrasonic cleaner water-bath seat 15, and purified liquid water 16, numerical control are added in sea water bath
The bath temperature of ultrasonic cleaner water-bath seat 15 is controlled by second temperature control knob 18, the power of ultrasonic wave transmitting module 14 by
Power control knob 17 is controlled and is adjusted；Addition funnel 3, condensation reflux device are set gradually from left to right on the top of three-necked flask 2
5, temperature inductor 6；3 lower part of addition funnel is equipped with liquid feeding control valve 4, and is fixed by addition funnel fixed frame 9；Condensation reflux device
5 are fixed by condensation reflux device control cage 10；Temperature inductor 6 is fixed by inductor fixed mount 7；Change to be in situ in three-necked flask 2
Property prepares nano silicon dioxide composite antioxidant mixed liquor 8.
Fig. 3 be it is in-situ modified prepare nano silicon dioxide composite antioxidant microscopic appearance figure, it is visible in figure：Nanometer titanium dioxide
Silicon face pattern whole smooth is mellow and full, uniform particle sizes are full, and grain size is in monodisperse status between 80-120nm.
Fig. 4 is the in-situ modified thermal weight loss collection of illustrative plates for preparing nano silicon dioxide composite antioxidant and pure antioxidant 1330, right
Than the weightless temperature in figure as it can be seen that the temperature of initial decomposition of nano silicon dioxide composite antioxidant is delayed, weightless temperature is obviously high
In pure antioxidant 1330, thermal stability improves.
Claims (2)
1. a kind of in-situ modified method for preparing nano silicon dioxide composite antioxidant, which is characterized in that the chemical substance used
Material is：Ethyl orthosilicate, the ammonium hydroxide for calculating a concentration of 25% based on mass fraction, absolute ethyl alcohol, acetone, antioxidant 1330, go from
Sub- water, the liquid chemical substance material utilization amount are calculated with volume parts；Wherein, the basic chemical property of antioxidant 1330 is such as
Under：
Chemical name：1,3,5- trimethyls -2,4,6- three (3,5- di-t-butyl -4- hydroxyls benzyl) benzene
Molecular formula：C54H78O3
Molecular weight：775.2
Molecular structural formula：
Preparation method is as follows：
(1) selected each chemical substance material
(2) in-situ modified to prepare nano silicon dioxide composite antioxidant
1. preparing solution
49 ~ 51 parts of absolute ethyl alcohols are measured, are placed in beaker for use；It measures 24 ~ 36 parts of ammonium hydroxide and is placed in the conical flask with rubber stopper
In it is for use；5.0-5.2 parts of ethyl orthosilicate and 49-51 parts of absolute ethyl alcohol are measured, is placed in beaker and mixes, stirred with glass bar
Mixing keeps it for use after mixing；It measures antioxidant 1330 to be dissolved in 145-150 parts of acetone, stirs evenly and be prepared into third
Quality-volume ratio of ketone solution, antioxidant 1330 and acetone is 8 ~ 10：29~30mg/ml；It is placed in until completely dissolved with glass
It is for use in the conical flask of glass plug；
2. in-situ modified prepare nano silicon dioxide composite antioxidant process
Absolute ethyl alcohol and ammonia spirit are placed in three-necked flask, are subsequently placed in magnetic agitation heating mantle, turn on agitator is opened
Heating is opened, sets agitator speed as 200r/min, warm temperature is set as 65 DEG C, configures condensation reflux unit；In temperature raising period
Between when temperature reaches 45 DEG C, with the speed of 0.75 part/min will teos solution be added three-necked flask in；Condensing reflux
After reacting 1h, acetone soln is added drop-wise in three-necked flask with the speed of 0.25 part/min；Condensing reflux reacts 6h；
3. ultrasonic water bath dispersion reaction
Three-necked flask 2. after reaction, is placed in ultrasonic water bath pond that the reaction was continued by step, and bath temperature is 60 DEG C, supersonic frequency
Rate is 80KHz, power 90W, reaction time 2h；
4. washing filters
By step, 3. reaction mixture is placed in beaker, and 100-150 parts of absolute ethyl alcohol is added, and 3min is stirred, at cleaning solution；It will washing
Liquid filters to obtain filter cake, and filter cake is placed in 200-250 parts of absolute ethyl alcohols, cleaning solution is stirred into, and filters；It so carries out 5 times, obtains
To filter cake；
Filter cake is added in 200 parts of deionized waters, agitator treating 5min, at cleaning solution；Filtering and washing to filtrate is in neutrality, and obtains
Product cake；
5. drying is ground up, sieved
By step, 4. products therefrom filter cake is placed in vacuum drying chamber dry, 60 DEG C, vacuum degree 0.1MPa of drying temperature, when dry
Between 2h；
Powder after drying agate mortar, pestle are ground, is then sieved with 400 mesh screens, obtains nanometer titanium dioxide
Silicon composite antioxidant product.
2. a kind of in-situ modified method for preparing nano silicon dioxide composite antioxidant according to claim 1, feature
It is, step（1）The chemical substance material that uses of preparation to be carried out selected, and carry out quality purity, concentration control：Positive silicic acid
Ethyl ester purity is 99.9%, absolute ethyl alcohol purity 99.9%；Acetone purity 99.9%；1330 purity 99.9% of antioxidant；Deionized water
Purity 99.9%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109326447A (en) * | 2018-11-07 | 2019-02-12 | 广州金立电子有限公司 | A kind of electrolytic capacitor |
| CN110328774A (en) * | 2019-07-15 | 2019-10-15 | 江苏极易新材料有限公司 | A kind of compound antioxidant granulating and forming new process |
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