CN109181105A - A kind of preparation method of modified grammite - Google Patents
A kind of preparation method of modified grammite Download PDFInfo
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- CN109181105A CN109181105A CN201810990037.1A CN201810990037A CN109181105A CN 109181105 A CN109181105 A CN 109181105A CN 201810990037 A CN201810990037 A CN 201810990037A CN 109181105 A CN109181105 A CN 109181105A
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- wollastonite
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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
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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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Abstract
The present invention relates to a kind of preparation methods of modified grammite, weigh a certain amount of EVA lotion, alpha-sulfo fatty acid methyl ester, deionized water, are put into reaction vessels, and reaction is stirred to react under room temperature, obtain solution A；It weighs a certain amount of solution A, wollastonite powder, calcium chloride, butyl glycol ether to be put into reaction vessels, lower reaction, cooling, filtering, dry modified grammite.It is better than with this technology synthesis modification wollastonite come improved polyalkene physical property and directly uses EVA rubber, wollastonite blending and modifying polyolefin, modified grammite can makes it spread more evenly across in polyolefin substrate as the effective carrier of wollastonite particle；Formd between wollastonite particle and EVA rubber certain it is special contain structure, this compound particle for containing structure is easier to play the synergistic effect of wollastonite particle and EVA rubber, makes polyolefin substrate that brittle-ductile transition occur, improve the physical property of polyolefin.
Description
Technical field
The invention belongs to technical field of polymer materials, particularly relate to a kind of preparation method of modified grammite.
Background technique
All the time, wollastonite is a kind of important filler of improved polyalkene, silicon ash as a kind of common inorganic filler
It is a kind of hot technology that recent studies in recent years developed that stone is polymer-modified.
A kind of new modified grammite of synthesis of the technical program innovation, it is available more excellent with its improved polyalkene
Different physical property, pertinent literature are simultaneously not found in report, this greatly expands the application field of wollastonite, have very real
Meaning.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of modified grammite, the modified silicon prepared by this preparation method
Lime stone can be improved the physical property of polyolefin.
The present invention is achieved by the following technical solutions:
A kind of preparation method of modified grammite, comprising the following steps:
(1) a certain amount of EVA lotion, alpha-sulfo fatty acid methyl ester, deionized water are weighed, is put into reaction vessels, room temperature
Lower reaction is stirred to react 1-3h, obtains solution A；
(2) it weighs a certain amount of solution A, wollastonite powder, calcium chloride, butyl glycol ether to be put into reaction vessels, 40-60
2-4h is reacted at DEG C, cooling, filtering, dry modified grammite.
The mass ratio of EVA lotion, alpha-sulfo fatty acid methyl ester, deionized water in step (1) is (400-600): (3-
5): (100-160).
The mass ratio of solution A, wollastonite powder, calcium chloride, butyl glycol ether in step (2) is (20-30): (60-
80): (1-3): (2-4).
The beneficial effects of the present invention are:
1, COO after EVA lotion and wollastonite mix, in EVA lotion-With the Ca on wollastonite surface2+Occur it is positive and negative from
Sub- bonding action, emulsion breaking simultaneously gathers the primary particle that wollastonite particle periphery forms a certain size, while silicon ash stone grain
The buffer action of son stablizes the partial size of modified grammite compound particle in particular range.
2, this technology creativeness has used calcium chloride, butyl glycol ether compounding to come as demulsifier, than single use chlorination
Calcium or butyl glycol ether effect will be got well.
3, it is better than directly come improved polyalkene physical property with EVA rubber, silicon ash with this technology synthesis modification wollastonite
Stone blending and modifying polyolefin, the reasons are as follows: 1. effective load of the modified grammite in the present invention as wollastonite particle
Body can be such that it spreads more evenly across in polyolefin substrate.2. it is special to form certain between wollastonite particle and EVA rubber
Contain structure, this compound particle for containing structure is easier to play the synergistic effect of wollastonite particle and EVA rubber, makes to gather
Brittle-ductile transition occurs for olefin substrate, improves the physical property of polyolefin.
Specific embodiment
Carry out the technical solution that the present invention will be described in detail by the following examples, embodiment below is merely exemplary, only
It can be used to explanation and illustration technical solution of the present invention, and be not to be construed as the limitation to technical solution of the present invention.
Raw material used in embodiments herein is as follows:
EVA lotion, laboratory are provided for oneself；Alpha-sulfo fatty acid methyl ester, Shandong Bao Lilai company；Deionized water, Shanghai joint-trial
Chemical reagent Co., Ltd；Wollastonite powder, Xinyu Dong Hui mining industry Co., Ltd；Calcium chloride, dragon Xinghua, Langfang Asia-Pacific work are limited
Company；Butyl glycol ether, Jinan Wen Tai Chemical Co., Ltd.；PBT (model 2002U), Polyplastics；PP (model Z30S), cyclopentadienyl
Name petrochemical industry；PE (model 5070), Panjin ethylene；PET (model PJ002), Yi Siman chemistry；PS (model 350), state of Taiwan Province
It is tall.
Test equipment used herein is as follows:
ZSK30 type double screw extruder, German W&P company；JL-1000 type tensile testing machine, the wide just experiment instrument in Guangzhou
The production of device company；HTL900-T-5B type injection (mo(u)lding) machine, the production of Hai Tai plastics machinery Co., Ltd；XCJ-500 type shock-testing
Machine, the production of Chengde testing machine factory；QT-1196 type tester for elongation, Dongguan City Gao Tai detecting instrument Co., Ltd；QD-GJS-
B12K type high-speed mixer, Beijing perseverance Order instrument and meter Co., Ltd.
The application provides a kind of preparation method of modified grammite, comprising the following steps:
(1) a certain amount of EVA lotion, alpha-sulfo fatty acid methyl ester, deionized water are weighed, is put into reaction vessels, room temperature
Lower reaction is stirred to react 1-3h, obtains solution A；EVA lotion, alpha-sulfo fatty acid methyl ester, deionized water mass ratio be (400-
600): (3-5): (100-160).
(2) it weighs a certain amount of solution A, wollastonite powder, calcium chloride, butyl glycol ether to be put into reaction vessels, 40-60
2-4h is reacted at DEG C, cooling, filtering, dry modified grammite.
The mass ratio of solution A, wollastonite powder, calcium chloride, butyl glycol ether in step (2) is (20-30): (60-
80): (1-3): (2-4).
Embodiment 1
(1) 4kg ethylene-vinyl acetate emulsion (EVA lotion), 30g alpha-sulfo fatty acid methyl ester, 1kg deionization are weighed
Water is put into reaction vessels, and reaction is stirred to react 1h under room temperature, obtains solution A.
(2) 200g solution A, 600g wollastonite powder, 10g calcium chloride, 20g butyl glycol ether are weighed and is put into reaction vessels
In, 2h is reacted at 40 DEG C, cooling, filtering, dry modified grammite P1.
Application examples 1
It takes 20 parts of P1 to be added in 80 parts of polypropylene (PP), stirs 10min through high mixer, be subsequently added into double screw extruder
Middle carry out blending extrusion, obtains PP composite material X1.
Wherein, double screw extruder includes six humidity provinces sequentially arranged, and the temperature of the first humidity province is 170 DEG C, the
The temperature of two humidity provinces is 220 DEG C, and the temperature of third humidity province is 230 DEG C, and the temperature of the 4th humidity province is 240 DEG C, the 5th temperature
The temperature for spending area is 240 DEG C, and the temperature of the 6th humidity province is 240 DEG C, and the head temperature of double screw extruder is 230 DEG C, screw rod
Revolving speed is 220r/min.
Comparative example 1
It takes 20 parts of wollastonites to be added in 80 parts of polypropylene (PP), stirs 10min through high mixer, be subsequently added into twin-screw and squeeze
Blending extrusion is carried out in machine out, obtains wollastonite/PP composite material D1.
Batten, properties of product data are made with injection molding machine in PP composite material prepared by above application examples 1 and comparative example 1
It is as shown in the table:
As can be seen from the above table:
The tensile strength of X1, bending strength, cantilever beam impact strength ratio D1 it is big, this illustrates that modified grammite is added
MODIFIED PP is more preferable than the physical property that commercially available wollastonite is added merely.
Embodiment 2
(1) weigh 6kg ethylene-vinyl acetate emulsion (EVA lotion), 50g alpha-sulfo fatty acid methyl ester, 1.6kg go from
Sub- water, is put into reaction vessels, and reaction is stirred to react 3h under room temperature, obtains solution A.
(2) 300g solution A, 800g wollastonite powder, 30g calcium chloride, 40g butyl glycol ether are weighed and is put into reaction vessels
In, 4h is reacted at 60 DEG C, cooling, filtering, dry modified grammite P2.
Application examples 2
It takes 20 parts of P2 to be added in 80 parts of polybutylene terephthalate (PBT)s (PBT), stirs 10min through high mixer, then
Carry out blending extrusion is added twin-screw extrude, PBT composite X2 is obtained.
Wherein, double screw extruder includes six humidity provinces sequentially arranged, and the temperature of the first humidity province is 200 DEG C, the
The temperature of two humidity provinces is 260 DEG C, and the temperature of third humidity province is 260 DEG C, and the temperature of the 4th humidity province is 260 DEG C, the 5th temperature
The temperature for spending area is 260 DEG C, and the temperature of the 6th humidity province is 260 DEG C, and the head temperature of double screw extruder is 260 DEG C, screw rod
Revolving speed is 300r/min.
Comparative example 2
It takes 20 parts of wollastonites to be added in 80 parts of PBT, stirs 10min through high mixer, be subsequently added into double screw extruder
Blending extrusion is carried out, wollastonite/PBT composite D2 is obtained.
Batten, properties of product number is made with injection molding machine in PBT composite prepared by above application examples 2 and comparative example 2
According to as shown in the table:
As can be seen from the above table:
The tensile strength of X2, bending strength, cantilever beam impact strength ratio D2 it is big, this illustrates that modified grammite is added
Modified PBT is more preferable than the physical property that commercially available wollastonite is added merely.
Embodiment 3
(1) weigh 5kg ethylene-vinyl acetate emulsion (EVA lotion), 40g alpha-sulfo fatty acid methyl ester, 1.3kg go from
Sub- water, is put into reaction vessels, and reaction is stirred to react 2h under room temperature, obtains solution A.
(2) 250g solution A, 700g wollastonite powder, 20g calcium chloride, 30g butyl glycol ether are weighed and is put into reaction vessels
In, 3h is reacted at 50 DEG C, cooling, filtering, dry modified grammite P3.
Application examples 3
It takes 20 parts of P3 to be added in 80 parts of polyethylene (PE), stirs 10min through high mixer, be subsequently added into double screw extruder
Middle carry out blending extrusion, obtains PE composite material X3.
Wherein, double screw extruder includes six humidity provinces sequentially arranged, and the temperature of the first humidity province is 120 DEG C, the
The temperature of two humidity provinces is 180 DEG C, and the temperature of third humidity province is 180 DEG C, and the temperature of the 4th humidity province is 180 DEG C, the 5th temperature
The temperature for spending area is 180 DEG C, and the temperature of the 6th humidity province is 180 DEG C, and the head temperature of double screw extruder is 180 DEG C, screw rod
Revolving speed is 300r/min.
Comparative example 3
It takes 20 parts of wollastonites in powder to be added in 80 parts of PE, stirs 10min through high mixer, be subsequently added into double screw extruder
Blending extrusion is carried out, wollastonite/PE composite material D3 is obtained.
Batten, properties of product data are made with injection molding machine in PE composite material prepared by above application examples 3 and comparative example 3
It is as shown in the table:
As can be seen from the above table:
The tensile strength of X3, bending strength, cantilever beam impact strength ratio D3 it is big, this illustrates that modified grammite is added
Modified PE is more preferable than the physical property that commercially available wollastonite is added merely.
Embodiment 4
(1) 4.3kg ethylene-vinyl acetate emulsion (EVA lotion), 35g alpha-sulfo fatty acid methyl ester, 1.2kg is weighed to go
Ionized water is put into reaction vessels, and reaction is stirred to react 1h under room temperature, obtains solution A.
(2) 250g solution A, 720g wollastonite powder, 25g calcium chloride, 25g butyl glycol ether are weighed and is put into reaction vessels
In, 4h is reacted at 40 DEG C, cooling, filtering, dry modified grammite P4.
Application examples 4
Take 20 parts of P4 to be added in 80 parts of polyethylene terephthalate (PET), stir 10min through high mixer, then plus
Enter and carry out blending extrusion in double screw extruder, obtains PET composite material X4.
Wherein, double screw extruder includes six humidity provinces sequentially arranged, and the temperature of the first humidity province is 260 DEG C, the
The temperature of two humidity provinces is 280 DEG C, and the temperature of third humidity province is 280 DEG C, and the temperature of the 4th humidity province is 280 DEG C, the 5th temperature
The temperature for spending area is 280 DEG C, and the temperature of the 6th humidity province is 280 DEG C, and the head temperature of double screw extruder is 280 DEG C, screw rod
Revolving speed is 320r/min.
Comparative example 4
It takes 20 parts of wollastonites in powder to be added in 80 parts of PET, stirs 10min through high mixer, be subsequently added into double screw extruder
Middle carry out blending extrusion, obtains wollastonite/PET composite material D4.
Batten, properties of product number is made with injection molding machine in PET composite material prepared by above application examples 4 and comparative example 4
According to as shown in the table:
As can be seen from the above table:
The tensile strength of X4, bending strength, cantilever beam impact strength ratio D4 it is big, this illustrates that modified grammite is added
Powder modified PET is more preferable than the physical property that commercially available wollastonite in powder is added merely.
Embodiment 5
(1) 4.2kg ethylene-vinyl acetate emulsion (EVA lotion), 38g alpha-sulfo fatty acid methyl ester, 1.1kg is weighed to go
Ionized water is put into reaction vessels, and reaction is stirred to react 1h under room temperature, obtains solution A.
(2) 260g solution A, 720g wollastonite powder, 15g calcium chloride, 35g butyl glycol ether are weighed and is put into reaction vessels
In, 2h is reacted at 60 DEG C, cooling, filtering, dry modified grammite P5.
Application examples 5
It takes 20 parts of P5 to be added in 80 parts of styrene (PS), stirs 10min through high mixer, be subsequently added into double screw extruder
Middle carry out blending extrusion, obtains PS composite material X5.
Wherein, double screw extruder includes six humidity provinces sequentially arranged, and the temperature of the first humidity province is 160 DEG C, the
The temperature of two humidity provinces is 200 DEG C, and the temperature of third humidity province is 200 DEG C, and the temperature of the 4th humidity province is 200 DEG C, the 5th temperature
The temperature for spending area is 200 DEG C, and the temperature of the 6th humidity province is 200 DEG C, and the head temperature of double screw extruder is 200 DEG C, screw rod
Revolving speed is 280r/min.
Comparative example 5
It takes 20 parts of wollastonites in powder to be added in 80 parts of PS, stirs 10min through high mixer, be subsequently added into double screw extruder
Blending extrusion is carried out, wollastonite/PS composite material D5 is obtained.
Batten, properties of product data are made with injection molding machine in PS composite material prepared by above application examples 5 and comparative example 5
It is as shown in the table:
As can be seen from the above table:
The tensile strength of X5, bending strength, cantilever beam impact strength ratio D5 it is big, this illustrates that modified grammite is added
The physical property that commercially available wollastonite in powder is added merely in the modified PS ratio of powder is more preferable.
This technology describes a kind of preparation method of modified wollastonite powder, and polyolefine material obtained is in physical property side
Face is also improved to some extent, this greatly expands the application field of composite polyolefine material, has very important significance.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And deformation, the scope of the present invention are extremely equally limited by appended claims.
Claims (3)
1. a kind of preparation method of modified grammite, which comprises the following steps:
(1) a certain amount of EVA lotion, alpha-sulfo fatty acid methyl ester, deionized water are weighed, is put into reaction vessels, it is anti-under room temperature
It should be stirred to react 1-3h, obtain solution A；
(2) it weighs a certain amount of solution A, wollastonite powder, calcium chloride, butyl glycol ether to be put into reaction vessels, at 40-60 DEG C
2-4h is reacted, cooling, filtering, dry modified grammite.
2. the preparation method of modified grammite according to claim 1, which is characterized in that EVA lotion in step (1),
Alpha-sulfo fatty acid methyl ester, deionized water mass ratio be (400-600): (3-5): (100-160).
3. the preparation method of modified grammite according to claim 1, which is characterized in that solution A, silicon in step (2)
Lime stone powder, calcium chloride, butyl glycol ether mass ratio be (20-30): (60-80): (1-3): (2-4).
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| CN201810990037.1A CN109181105B (en) | 2018-08-28 | 2018-08-28 | Preparation method of modified wollastonite |
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| CN201810990037.1A CN109181105B (en) | 2018-08-28 | 2018-08-28 | Preparation method of modified wollastonite |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106479073A (en) * | 2016-10-21 | 2017-03-08 | 安徽江淮汽车集团股份有限公司 | A kind of anti-static and abrasion-resistant high-performance PS composite and preparation method thereof |
| CN107418050A (en) * | 2017-06-21 | 2017-12-01 | 安徽江淮汽车集团股份有限公司 | A kind of high-performance antibiosis PP PA6 composites and preparation method thereof |
| CN107417974A (en) * | 2017-06-21 | 2017-12-01 | 安徽江淮汽车集团股份有限公司 | A kind of modified micaceous powder and preparation method thereof |
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2018
- 2018-08-28 CN CN201810990037.1A patent/CN109181105B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106479073A (en) * | 2016-10-21 | 2017-03-08 | 安徽江淮汽车集团股份有限公司 | A kind of anti-static and abrasion-resistant high-performance PS composite and preparation method thereof |
| CN107418050A (en) * | 2017-06-21 | 2017-12-01 | 安徽江淮汽车集团股份有限公司 | A kind of high-performance antibiosis PP PA6 composites and preparation method thereof |
| CN107417974A (en) * | 2017-06-21 | 2017-12-01 | 安徽江淮汽车集团股份有限公司 | A kind of modified micaceous powder and preparation method thereof |
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