CN109111634A - A kind of preparation method being alkylated superfine talcum powder modified poly ethylene - Google Patents
A kind of preparation method being alkylated superfine talcum powder modified poly ethylene Download PDFInfo
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- CN109111634A CN109111634A CN201810952160.4A CN201810952160A CN109111634A CN 109111634 A CN109111634 A CN 109111634A CN 201810952160 A CN201810952160 A CN 201810952160A CN 109111634 A CN109111634 A CN 109111634A
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- talcum powder
- superfine talcum
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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
- C08K9/10—Encapsulated ingredients
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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
- C08K3/34—Silicon-containing compounds
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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
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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
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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Abstract
The invention belongs to modified powder field of material preparation, and in particular to a kind of preparation method for being alkylated superfine talcum powder modified poly ethylene.The present invention is alkylated modification to superfine talcum powder surface using the alkylsilanol of gas phase, and this alkyl-modified powder and polyvinyl resin melting mixing are granulated, and the ultra-fine sliding modified poly ethylene of alkylation is made.Modified poly ethylene is prepared using this alkylation superfine talcum powder, the mechanical strength and heat resistance of polyethylene significantly improve.
Description
Technical field
The invention belongs to powder-modified field of material preparation, and in particular to a kind of alkylation superfine talcum powder modified poly ethylene
Preparation method.
Background technique
Talcum powder is cheap, is usually used in the filling-modified of polythene material.The main component of talcum powder is britesorb,
It is low with the interface interaction intensity of polythene material with stronger polarity and hygroscopicity, it directly melts mixture and is unable to reach well
Using effect.The activating substances such as silane are generally attached to talcum powder surface by the way of liquid-solid mixing by the prior art, are come
Improve the compatibility of talcum powder and polyvinyl resin.Superfine talcum powder and nano talc of the granularity less than 6.5 μm (2000 mesh)
With significant building-up effect, it will largely block the immersion and attachment of liquid activator.By talcum powder partial size and liquid-solid leaching
Moisten the influence of effect, degree of adhesion is generally difficult to control, is difficult for activator to be evenly affixed to talcum powder surface comprehensively.Currently,
The method for preparing activated talc powder is more, and activator mostly realizes attachment with liquid-solid technology mode, and adhesion effect is general.This
This liquid-solid attachment preparation thinking has been abandoned in invention, is prepared for surface by gas-solid technology mode and is distributed uniform alkyl comprehensively
Change superfine talcum powder, and using this alkylation superfine talcum powder and polyvinyl resin melt blending, preparation is alkylated ultra-fine cunning
Mountain flour modified poly ethylene.
Summary of the invention
The technical scheme is that the shortcoming in order to overcome prior art, provides a kind of alkylation superfine talcum powder
The preparation method of modified poly ethylene.
The invention proposes a kind of preparation methods for being alkylated superfine talcum powder modified poly ethylene, include the following steps:
1) superfine talcum powder powder is added in seal-off pressure reactor, ultrasound and heated under vacuum 30-60min；
2) vacuum is closed, is passed through alkylsilanol steam, pressure maintaining 0.4-0.6MPa heats 10- under ultrasound and stirring condition
15min；
3) stop alkylsilanol steam to be passed through, maintain ultrasound and stirring, continue to heat 10-15min；
4) stop heating and stirring, maintain ultrasound condition, vacuum detaches 20min；
5) stirring and ultrasound are closed, is discharged after cooling, alkylation superfine talcum powder is made；
6) alkylation superfine talcum powder is pre-mixed with polyvinyl resin, melting mixing is granulated at 170-180 DEG C, alkyl
Change the 5-10wt% that superfine talcum powder accounts for total content, the ultra-fine sliding modified poly ethylene of alkylation is made.
Wherein, superfine talcum powder partial size≤6.5 μm.
Wherein, the alkylsilanol is one of methyl silanol, dimethyl silanols, trimethyl silanol.
Wherein, step 1), 2) and 3) described in heating temperature be 120-130 DEG C.
Wherein, step 1), 2), 3) He 4) described in ultrasound condition be power be 100-200W.
Wherein, step 1) and 4) described in vacuum condition be vacuum degree be 20-25kPa.
Wherein, step 2) and 3) described in mixing speed be 150-300rpm.
The present invention is alkylated modification to superfine talcum powder surface using the alkylsilanol of gas phase, and this alkyl is changed
Property powder and polyvinyl resin melting mixing be granulated, the ultra-fine sliding modified poly ethylene of alkylation is made.Firstly, in vacuum and certain temperature
The lower free state water and volatile matter for removing talcum powder surface of degree.Then alkylsilanol is passed through reactor in the form of high pressure gas
In, gaseous state-solid-state comprehensive engagement is formed with superfine talcum powder and is reacted.By ultrasound, stirring and vapour pressure effect, promote gas-
Solid interface update and contact, alkylsilanol gaseous molecular forms attachment and anti-completely into powder gap, on talcum powder surface
It answers.Finally, the free state silanol being removed in vacuum between powder surface and gap.It discharges after cooling in reactor, alkylation is made
Superfine talcum powder.Superfine talcum powder will be alkylated and polyvinyl resin is granulated in 170-180 DEG C of melting mixing, and obtain alkylation
Ultra-fine sliding modified poly ethylene.
Beneficial effects of the present invention: this method is alkylated modification, phase to talcum powder surface using gaseous state alkylsilanol
Than in existing liquid-solid mixed silanization treatment technology, the present invention can utmostly avoid activator in the nothing of powder surface
Accumulation is imitated, alkyl activation efficiency is improved, obtained surface attachment is more complete orderly.The temperature as defined in this technology and pressure
Under power, superfine powder surface is completely covered in alkylsilanol molecular film, and sufficiently reacts, and realizes comprehensive alkane on superfine talcum powder surface
Base, and then superfine talcum powder is obviously improved to the interface affinity of polyvinyl resin.Using this alkylation superfine talcum powder
Modified poly ethylene is prepared, the mechanical strength and heat resistance of polyethylene are remarkably improved.
Specific embodiment
Below with reference to embodiment, the present invention is further illustrated.
Embodiment 1
1) 6.5 μm of partial size of superfine talcum powder powder is added in seal-off pressure reactor, is added under ultrasound and vacuum condition
Hot 45min, ultrasonic power 100W, vacuum degree 25kPa, 120 DEG C of heating temperature；
2) vacuum is closed, is passed through methyl silanol steam, pressure maintaining 0.4MPa heats 10min under ultrasound and stirring condition, ultrasound
Power 100W, mixing speed 150rpm, 120 DEG C of heating temperature；
3) stop methyl silanol steam to be passed through, maintain ultrasound and stirring, continue to heat 10min；
4) stop heating and stirring, maintain ultrasound condition, vacuum detaches 20min, vacuum degree 25kPa；
5) stirring and ultrasound are closed, is discharged after cooling, alkylation superfine talcum powder is made；
6) alkylation superfine talcum powder is pre-mixed with polyvinyl resin, melting mixing is granulated at 170-180 DEG C, alkyl
Change superfine talcum powder and account for the 5% of total content, the ultra-fine sliding modified poly ethylene of alkylation is made, the used polyethylene trade mark is
DFDA7042。
Embodiment 2
1) 6.5 μm of partial size of superfine talcum powder powder is added in seal-off pressure reactor, is added under ultrasound and vacuum condition
Hot 45min, ultrasonic power 200W, vacuum degree 25kPa, 130 DEG C of heating temperature；
2) vacuum is closed, is passed through methyl silanol steam, pressure maintaining 0.6MPa heats 15min under ultrasound and stirring condition, ultrasound
Power 200W, mixing speed 300rpm, 130 DEG C of heating temperature；
3) stop methyl silanol steam to be passed through, maintain ultrasound and stirring, continue to heat 15min；
4) stop heating and stirring, maintain ultrasound condition, vacuum detaches 20min, vacuum degree 25kPa；
5) stirring and ultrasound are closed, is discharged after cooling, alkylation superfine talcum powder is made.
6) alkylation superfine talcum powder is pre-mixed with polyvinyl resin, melting mixing is granulated at 170-180 DEG C, alkyl
Change superfine talcum powder and account for the 10% of total content, the ultra-fine sliding modified poly ethylene of alkylation is made, the used polyethylene trade mark is
DFDA7042。
Embodiment 3
1) 6.5 μm of partial size of superfine talcum powder powder is added in seal-off pressure reactor, is added under ultrasound and vacuum condition
Hot 60min, ultrasonic power 100W, vacuum degree 20kPa, 130 DEG C of heating temperature；
2) vacuum is closed, is passed through trimethyl silanol steam, pressure maintaining 0.6MPa heats 15min under ultrasound and stirring condition, surpasses
Acoustical power 200W, mixing speed 300rpm, 130 DEG C of heating temperature；
3) stop trimethyl silanol steam to be passed through, maintain ultrasound and stirring, continue to heat 15min；
4) stop heating and stirring, maintain ultrasound condition, vacuum detaches 20min, vacuum degree 20kPa；
5) stirring and ultrasound are closed, is discharged after cooling, alkylation superfine talcum powder is made.
6) alkylation superfine talcum powder is pre-mixed with polyvinyl resin, melting mixing is granulated at 170-180 DEG C, alkyl
Change superfine talcum powder and account for the 10% of total content, the ultra-fine sliding modified poly ethylene of alkylation is made, the used polyethylene trade mark is
R50035。
Embodiment 4
1) 1.6 μm of partial size of superfine talcum powder powder is added in seal-off pressure reactor, is added under ultrasound and vacuum condition
Hot 60min, ultrasonic power 150W, vacuum degree 20kPa, 130 DEG C of heating temperature；
2) vacuum is closed, is passed through dimethyl silanols steam, pressure maintaining 0.5MPa heats 15min under ultrasound and stirring condition, surpasses
Acoustical power 150W, mixing speed 300rpm, 130 DEG C of heating temperature；
3) stop dimethyl silanols steam to be passed through, maintain ultrasound and stirring, continue to heat 15min；
4) stop heating and stirring, maintain ultrasound condition, vacuum detaches 20min, vacuum degree 20kPa；
5) stirring and ultrasound are closed, is discharged after cooling, alkylation superfine talcum powder is made.
6) alkylation superfine talcum powder is pre-mixed with polyvinyl resin, melting mixing is granulated at 170-180 DEG C, alkyl
Change superfine talcum powder and account for the 10% of total content, the ultra-fine sliding modified poly ethylene of alkylation is made, the used polyethylene trade mark is
R50035。
Embodiment 5
1) 0.8 μm of partial size of superfine talcum powder powder is added in seal-off pressure reactor, is added under ultrasound and vacuum condition
Hot 60min, ultrasonic power 200W, vacuum degree 20kPa, 130 DEG C of heating temperature；
2) vacuum is closed, is passed through trimethyl silanol steam, pressure maintaining 0.6MPa heats 15min under ultrasound and stirring condition, surpasses
Acoustical power 200W, mixing speed 300rpm, 130 DEG C of heating temperature；
3) stop trimethyl silanol steam to be passed through, maintain ultrasound and stirring, continue to heat 15min；
4) stop heating and stirring, maintain ultrasound condition, vacuum detaches 20min, vacuum degree 20kPa；
5) stirring and ultrasound are closed, is discharged after cooling, alkylation superfine talcum powder is made.
6) alkylation superfine talcum powder is pre-mixed with polyvinyl resin, melting mixing is granulated at 170-180 DEG C, alkyl
Change superfine talcum powder and account for the 10% of total content, the ultra-fine sliding modified poly ethylene of alkylation is made, the used polyethylene trade mark is
DMDA8008。
Embodiment 6
1) 0.8 μm of talcum powder of partial size is added in seal-off pressure reactor, ultrasound and cooling after heated under vacuum 1h
To room temperature, ultrasonic power 200W, vacuum degree 25kPa；
2) trimethyl silanol of 1% talcum powder parts by weight is added；30min is stirred under ultrasound condition, is discharged, and alkyl is made
Change superfine talcum powder, ultrasonic power 200W, mixing speed 300rpm；
3) alkylation superfine talcum powder is pre-mixed with polyvinyl resin, melting mixing is granulated at 170-180 DEG C, alkyl
Change superfine talcum powder and account for the 10% of total content, the ultra-fine sliding modified poly ethylene of alkylation is made, the used polyethylene trade mark is
DMDA8008。
In the present embodiment, it is the liquid-solid attachment under normal temperature and pressure that alkylation superfine talcum powder, which prepares attached form,.
Embodiment 7
1) 0.8 μm of talcum powder of partial size is added in seal-off pressure reactor, ultrasound and heated under vacuum 1h, ultrasonic function
Rate 200W, vacuum degree 25kPa；
2) vacuum is closed, the trimethyl silanol of 1% talcum powder parts by weight is added, opens return valve, ultrasound and stirring condition
Lower heating 30min, ultrasonic power 200W, mixing speed 300rpm, 130 DEG C of heating temperature；
3) stirring and ultrasound are closed, is discharged after cooling, alkylation superfine talcum powder is made.
4) alkylation superfine talcum powder is pre-mixed with polyvinyl resin, melting mixing is granulated at 170-180 DEG C, alkyl
Change superfine talcum powder and account for the 10% of total content, the ultra-fine sliding modified poly ethylene of alkylation is made, the used polyethylene trade mark is
DMDA8008。
In the present embodiment, alkylation superfine talcum powder preparation form is the gas-solid attachment under normal pressure.
Embodiment 8
1) 0.8 μm of partial size of superfine talcum powder powder is added in seal-off pressure reactor, heated under vacuum
60min, vacuum degree 20kPa, 130 DEG C of heating temperature；
2) vacuum is closed, is passed through trimethyl silanol steam, pressure maintaining 0.6MPa heats 15min, and 130 DEG C of heating temperature；
3) stop trimethyl silanol steam to be passed through, continue to heat 15min；
4) stop heating, vacuum detaches 20min, vacuum degree 20kPa；
5) it discharges after cooling, alkylation superfine talcum powder is made.
6) alkylation superfine talcum powder is pre-mixed with polyvinyl resin, melting mixing is granulated at 170-180 DEG C, alkyl
Change superfine talcum powder and account for the 10% of total content, the ultra-fine sliding modified poly ethylene of alkylation is made, the used polyethylene trade mark is
DMDA8008。
In the present embodiment, alkylation superfine talcum powder preparation process does not apply ultrasound and stirring.
Embodiment 9
Superfine talcum powder and polyvinyl resin are pre-mixed, melting mixing is granulated at 170-180 DEG C, and superfine talcum powder accounts for
The 10% of total content, is made superfine talcum powder modified poly ethylene, and the used polyethylene trade mark is DMDA8008.
In the present embodiment, superfine talcum powder partial size is 0.8 μm, is not alkylated modification.
It is prepared using injection molding process and detects sample, 170-190 DEG C of injection temperature, injection pressure 40-50MPa, pressure maintaining
Time 45s.Sample is detected after adjusting 48h under 23 DEG C of temperature, 45% environment of humidity.
Tensile property is detected by GB/T 1040.2-2006, tensile speed 50mm/min.
Vicat softening temperature is detected by GB/T 1633-2000.
Testing result see the table below.
Claims (7)
1. a kind of preparation method for being alkylated superfine talcum powder modified poly ethylene, which is characterized in that preparation method includes following step
It is rapid:
1) superfine talcum powder powder is added in seal-off pressure reactor, ultrasound and heated under vacuum 30-60min；
2) vacuum is closed, is passed through alkylsilanol steam, pressure maintaining 0.4-0.6MPa heats 10-15min under ultrasound and stirring condition；
3) stop alkylsilanol steam to be passed through, maintain ultrasound and stirring, continue to heat 10-15min；
4) stop heating and stirring, maintain ultrasound condition, vacuum detaches 20min；
5) stirring and ultrasound are closed, is discharged after cooling, alkylation superfine talcum powder is made；
6) alkylation superfine talcum powder is pre-mixed with polyvinyl resin, melting mixing is granulated at 170-180 DEG C, and alkylation is super
Fine and smooth mountain flour accounts for the 5-10wt% of total content, and the ultra-fine sliding modified poly ethylene of alkylation is made.
2. the method according to claim 1, wherein superfine talcum powder partial size≤6.5 μm.
3. the method according to claim 1, wherein the alkylsilanol be methyl silanol, dimethyl silanols,
One of trimethyl silanol.
4. the method according to claim 1, wherein step 1), 2) and 3) described in heating temperature be 120-130
℃。
5. the method according to claim 1, wherein step 1), 2), 3), 4) described in ultrasound condition be power
For 100-200W.
6. the method according to claim 1, wherein step 1) and 4) described in vacuum condition be that vacuum degree is
20-25kPa。
7. the method according to claim 1, wherein step 2) and 3) described in mixing speed be 150-
300rpm。
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| CN201810952160.4A CN109111634B (en) | 2018-08-06 | 2018-08-06 | Preparation method of alkylated superfine talcum powder modified polyethylene |
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| CN201810952160.4A CN109111634B (en) | 2018-08-06 | 2018-08-06 | Preparation method of alkylated superfine talcum powder modified polyethylene |
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| CN106398320A (en) * | 2016-08-31 | 2017-02-15 | 泉州市旭丰粉体原料有限公司 | Preparation method and application of high-modulus modified talcum powder |
-
2018
- 2018-08-06 CN CN201810952160.4A patent/CN109111634B/en active Active
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|---|---|---|---|---|
| JPS55155039A (en) * | 1979-05-22 | 1980-12-03 | Mitsubishi Petrochem Co Ltd | Cross-linking ethylene copolymer composition |
| US5403891A (en) * | 1993-07-01 | 1995-04-04 | Dow Corning Corporation | Organosilicon resin composition as thermoplastic resin lubricant |
| CN101501124A (en) * | 2006-08-03 | 2009-08-05 | 日产自动车株式会社 | Surface-coated aluminum oxide nanoparticle and resin composition thereof |
| CN102417202A (en) * | 2011-09-02 | 2012-04-18 | 中国日用化学工业研究院 | Vapor phase method for modifying nano zinc oxide |
| CN104974557A (en) * | 2015-07-10 | 2015-10-14 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for modifying ultrafine oxide powder by using supercritical carbon dioxide |
| CN106398320A (en) * | 2016-08-31 | 2017-02-15 | 泉州市旭丰粉体原料有限公司 | Preparation method and application of high-modulus modified talcum powder |
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