CN109181105B - Preparation method of modified wollastonite - Google Patents
Preparation method of modified wollastonite Download PDFInfo
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- CN109181105B CN109181105B CN201810990037.1A CN201810990037A CN109181105B CN 109181105 B CN109181105 B CN 109181105B CN 201810990037 A CN201810990037 A CN 201810990037A CN 109181105 B CN109181105 B CN 109181105B
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- 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
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Abstract
The invention relates to a preparation method of modified wollastonite, which comprises the steps of weighing a certain amount of EVA emulsion, α -sulfo fatty acid methyl ester and deionized water, placing the materials into a reaction vessel, reacting and stirring at normal temperature to react to obtain a solution A, weighing a certain amount of the solution A, wollastonite powder, calcium chloride and ethylene glycol monobutyl ether, placing the solution A, wollastonite powder, calcium chloride and ethylene glycol monobutyl ether into the reaction vessel, reacting, cooling, filtering and drying to obtain the modified wollastonite.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to a preparation method of modified wollastonite.
Background
Wollastonite, which is a commonly used inorganic filler, is an important filler for modified polyolefins, and wollastonite modified polymers are a popular technique developed in recent years.
The technical scheme innovatively synthesizes the novel modified wollastonite, the polyolefin modified by the wollastonite can obtain excellent physical properties, and related documents are not reported, so that the application field of the wollastonite is greatly expanded, and the wollastonite modified polyolefin has very practical significance.
Disclosure of Invention
The invention aims to provide a preparation method of modified wollastonite, and the modified wollastonite prepared by the preparation method can improve the physical properties of polyolefin.
The invention is realized by the following technical scheme:
a preparation method of modified wollastonite comprises the following steps:
(1) weighing a certain amount of EVA emulsion, α -sulfo fatty acid methyl ester and deionized water, putting the mixture into a reaction vessel, reacting and stirring at normal temperature for 1-3h to obtain a solution A;
(2) weighing a certain amount of the solution A, wollastonite powder, calcium chloride and ethylene glycol monobutyl ether, putting the solution A, the wollastonite powder, the calcium chloride and the ethylene glycol monobutyl ether into a reaction vessel, reacting for 2-4h at 40-60 ℃, cooling, filtering and drying to obtain the modified wollastonite.
The mass ratio of the EVA emulsion, α -sulfo fatty acid methyl ester and deionized water in the step (1) is (400-.
The mass ratio of the solution A, the wollastonite powder, the calcium chloride and the ethylene glycol monobutyl ether in the step (2) is (20-30): (60-80): (1-3): (2-4).
The invention has the beneficial effects that:
1. when the EVA emulsion and the wollastonite are mixed, the COO in the EVA emulsion-Ca with wollastonite surface2+The positive and negative ion bonding effect is generated, the emulsion is broken and gathered around the wollastonite particles to form primary particles with a certain size, and the particle size of the modified wollastonite composite particles is stabilized in a specific range by the isolation effect of the wollastonite particles.
2. The technology creatively uses the complex of calcium chloride and ethylene glycol monobutyl ether as the demulsifier, and has better effect than the single use of the calcium chloride or the ethylene glycol monobutyl ether.
3.① the modified wollastonite in this invention can be dispersed in polyolefin matrix more uniformly as effective carrier of wollastonite particle, ② wollastonite particle and EVA rubber form a special occlusion structure, the composite particle of this occlusion structure can exert the synergistic effect of wollastonite particle and EVA rubber more easily, make polyolefin matrix produce brittle and tough transformation, and improve the physical property of polyolefin.
Detailed Description
The technical solutions of the present invention are described in detail below by examples, and the following examples are only exemplary and can be used only for explaining and explaining the technical solutions of the present invention, but not construed as limiting the technical solutions of the present invention.
The raw materials used in the examples of the present application are as follows:
EVA emulsion, laboratory owned, α -sulfo fatty acid methyl ester, Shandong Baolilai, deionized water, Shanghai's joint test chemical reagent, wollastonite powder, Xinyuanchui mining Co., Ltd, calcium chloride, Gallery Atalane Daocheng chemical Co., Ltd, ethylene glycol butyl ether, Jinan Wentai chemical Co., Ltd, PBT (model 2002U), Nippon Baoji, PP (model Z30S), Mognonie, PE (model 5070), Spilain ethylene, PET (model PJ002), Issmann chemical, PS (model 350), Taiwan national Joe.
The test instrument used in this application is as follows:
the test device comprises a ZSK30 type double-screw extruder, Germany W & P company, a J L-1000 type tensile testing machine, a Guangzhou city Guangzhou experiment instrument company, a HT L900-T-5B type injection molding machine, a Haitai plastics machinery company, a XCJ-500 type impact testing machine, a Chengde test machine company, a QT-1196 type tensile testing instrument, a Gaotai detection instrument company, a QD-GJS-B12K type high-speed stirring machine, and a Beijing HengOlder instrument and instrument company, wherein the ZSK30 type double-screw extruder is produced by a Guangzhou city Goji experiment instrument company.
The application provides a preparation method of modified wollastonite, which comprises the following steps:
(1) weighing a certain amount of EVA emulsion, α -sulfo fatty acid methyl ester and deionized water, placing the mixture into a reaction vessel, reacting and stirring the mixture for 1 to 3 hours at normal temperature to obtain a solution A, wherein the mass ratio of the EVA emulsion to the α -sulfo fatty acid methyl ester to the deionized water is (400-) -600: 3-5: 100-.
(2) Weighing a certain amount of the solution A, wollastonite powder, calcium chloride and ethylene glycol monobutyl ether, putting the solution A, the wollastonite powder, the calcium chloride and the ethylene glycol monobutyl ether into a reaction vessel, reacting for 2-4h at 40-60 ℃, cooling, filtering and drying to obtain the modified wollastonite.
The mass ratio of the solution A, the wollastonite powder, the calcium chloride and the ethylene glycol monobutyl ether in the step (2) is (20-30): (60-80): (1-3): (2-4).
Example 1
(1) Weighing 4kg of ethylene-vinyl acetate emulsion (EVA emulsion), 30g of α -sulfo fatty acid methyl ester and 1kg of deionized water, putting the materials into a reaction vessel, and reacting and stirring the materials for 1 hour at normal temperature to obtain a solution A.
(2) Weighing 200g of the solution A, 600g of wollastonite powder, 10g of calcium chloride and 20g of ethylene glycol monobutyl ether, putting the mixture into a reaction vessel, reacting for 2 hours at 40 ℃, cooling, filtering and drying to obtain modified wollastonite P1.
Application example 1
And adding 20 parts of P1 into 80 Parts of Polypropylene (PP), stirring for 10min by a high-speed mixer, and then adding into a double-screw extruder for blending and extruding to obtain the PP composite material X1.
The double-screw extruder comprises six temperature zones which are sequentially arranged, wherein the temperature of the first temperature zone is 170 ℃, the temperature of the second temperature zone is 220 ℃, the temperature of the third temperature zone is 230 ℃, the temperature of the fourth temperature zone is 240 ℃, the temperature of the fifth temperature zone is 240 ℃, the temperature of the sixth temperature zone is 240 ℃, the head temperature of the double-screw extruder is 230 ℃, and the screw rotating speed is 220 r/min.
Comparative example 1
Adding 20 parts of wollastonite into 80 Parts of Polypropylene (PP), stirring for 10min by a high-speed mixer, and then adding into a double-screw extruder for blending and extruding to obtain the wollastonite/PP composite material D1.
The PP composite materials prepared in the application example 1 and the comparative example 1 are made into sample strips by an injection molding machine, and the product performance data are shown in the following table:
as can be seen from the above table:
the tensile strength, bending strength and Izod impact strength of X1 are higher than those of D1, which shows that the physical properties of PP modified by adding modified wollastonite are better than those of PP modified by adding only commercial wollastonite.
Example 2
(1) Weighing 6kg of ethylene-vinyl acetate emulsion (EVA emulsion), 50g of α -sulfo fatty acid methyl ester and 1.6kg of deionized water, putting the materials into a reaction vessel, and reacting and stirring the materials for reaction for 3 hours at normal temperature to obtain a solution A.
(2) And weighing 300g of the solution A, 800g of wollastonite powder, 30g of calcium chloride and 40g of ethylene glycol monobutyl ether, putting the mixture into a reaction vessel, reacting for 4 hours at the temperature of 60 ℃, cooling, filtering and drying to obtain the modified wollastonite P2.
Application example 2
And adding 20 parts of P2 into 80 parts of polybutylene terephthalate (PBT), stirring for 10min by a high-speed mixer, and then adding into a double-screw extruder for blending and extruding to obtain the PBT composite material X2.
The double-screw extruder comprises six temperature zones which are sequentially arranged, wherein the temperature of the first temperature zone is 200 ℃, the temperature of the second temperature zone is 260 ℃, the temperature of the third temperature zone is 260 ℃, the temperature of the fourth temperature zone is 260 ℃, the temperature of the fifth temperature zone is 260 ℃, the temperature of the sixth temperature zone is 260 ℃, the head temperature of the double-screw extruder is 260 ℃, and the screw rotating speed is 300 r/min.
Comparative example 2
And adding 20 parts of wollastonite into 80 parts of PBT, stirring for 10min by a high-speed mixer, and then adding into a double-screw extruder for blending and extruding to obtain the wollastonite/PBT composite material D2.
The PBT composite materials prepared in the application example 2 and the comparative example 2 are made into sample strips by an injection molding machine, and the product performance data are shown in the following table:
as can be seen from the above table:
the tensile strength, bending strength and Izod impact strength of X2 are higher than those of D2, which shows that the physical properties of the PBT modified by adding the modified wollastonite are better than those of the PBT modified by adding the commercial wollastonite only.
Example 3
(1) Weighing 5kg of ethylene-vinyl acetate emulsion (EVA emulsion), 40g of α -sulfo fatty acid methyl ester and 1.3kg of deionized water, putting the materials into a reaction vessel, and reacting and stirring the materials for 2 hours at normal temperature to obtain a solution A.
(2) Weighing 250g of the solution A, 700g of wollastonite powder, 20g of calcium chloride and 30g of ethylene glycol monobutyl ether, putting the mixture into a reaction vessel, reacting for 3 hours at 50 ℃, cooling, filtering and drying to obtain the modified wollastonite P3.
Application example 3
And adding 20 parts of P3 into 80 parts of Polyethylene (PE), stirring for 10min by a high-speed mixer, and then adding into a double-screw extruder for blending and extruding to obtain the PE composite material X3.
The double-screw extruder comprises six temperature zones which are sequentially arranged, wherein the temperature of the first temperature zone is 120 ℃, the temperature of the second temperature zone is 180 ℃, the temperature of the third temperature zone is 180 ℃, the temperature of the fourth temperature zone is 180 ℃, the temperature of the fifth temperature zone is 180 ℃, the temperature of the sixth temperature zone is 180 ℃, the head temperature of the double-screw extruder is 180 ℃, and the screw rotating speed is 300 r/min.
Comparative example 3
And adding 20 parts of wollastonite powder into 80 parts of PE, stirring for 10min by using a high-speed mixer, and then adding into a double-screw extruder for blending and extruding to obtain the wollastonite/PE composite material D3.
The PE composite materials prepared in application example 3 and comparative example 3 were molded into sample bars by an injection molding machine, and the product performance data are shown in the following table:
as can be seen from the above table:
the tensile strength, flexural strength and Izod impact strength of X3 were greater than those of D3, indicating that the physical properties of PE modified by adding modified wollastonite were better than those of PE modified by adding only commercial wollastonite.
Example 4
(1) Weighing 4.3kg of ethylene-vinyl acetate emulsion (EVA emulsion), 35g of α -sulfo fatty acid methyl ester and 1.2kg of deionized water, putting the mixture into a reaction vessel, and reacting and stirring the mixture for 1 hour at normal temperature to obtain a solution A.
(2) Weighing 250g of the solution A, 720g of wollastonite powder, 25g of calcium chloride and 25g of ethylene glycol monobutyl ether, putting the mixture into a reaction vessel, reacting for 4 hours at 40 ℃, cooling, filtering and drying to obtain the modified wollastonite P4.
Application example 4
Adding 20 parts of P4 into 80 parts of polyethylene terephthalate (PET), stirring for 10min by a high-speed mixer, and then adding into a double-screw extruder for blending and extruding to obtain the PET composite material X4.
The double-screw extruder comprises six temperature zones which are sequentially arranged, wherein the temperature of the first temperature zone is 260 ℃, the temperature of the second temperature zone is 280 ℃, the temperature of the third temperature zone is 280 ℃, the temperature of the fourth temperature zone is 280 ℃, the temperature of the fifth temperature zone is 280 ℃, the temperature of the sixth temperature zone is 280 ℃, the head temperature of the double-screw extruder is 280 ℃, and the screw rotating speed is 320 r/min.
Comparative example 4
And adding 20 parts of wollastonite powder into 80 parts of PET, stirring for 10min by using a high-speed mixer, and then adding into a double-screw extruder for blending and extruding to obtain the wollastonite/PET composite material D4.
The PET composite materials prepared in application example 4 and comparative example 4 were molded into sample bars by an injection molding machine, and the product performance data are shown in the following table:
as can be seen from the above table:
the tensile strength, flexural strength and Izod impact strength of X4 were greater than those of D4, indicating that the physical properties of PET modified with the addition of modified wollastonite powder were better than those of PET modified with the addition of commercial wollastonite powder alone.
Example 5
(1) Weighing 4.2kg of ethylene-vinyl acetate emulsion (EVA emulsion), 38g of α -sulfo fatty acid methyl ester and 1.1kg of deionized water, putting the materials into a reaction vessel, and reacting and stirring the materials for 1 hour at normal temperature to obtain a solution A.
(2) 260g of the solution A, 720g of wollastonite powder, 15g of calcium chloride and 35g of ethylene glycol monobutyl ether are weighed and put into a reaction vessel to react for 2 hours at the temperature of 60 ℃, and the modified wollastonite P5 is obtained after cooling, filtering and drying.
Application example 5
And adding 20 parts of P5 into 80 Parts of Styrene (PS), stirring for 10min by a high-speed mixer, and then adding into a double-screw extruder for blending and extruding to obtain the PS composite material X5.
The double-screw extruder comprises six temperature zones which are sequentially arranged, wherein the temperature of the first temperature zone is 160 ℃, the temperature of the second temperature zone is 200 ℃, the temperature of the third temperature zone is 200 ℃, the temperature of the fourth temperature zone is 200 ℃, the temperature of the fifth temperature zone is 200 ℃, the temperature of the sixth temperature zone is 200 ℃, the head temperature of the double-screw extruder is 200 ℃, and the screw rotating speed is 280 r/min.
Comparative example 5
And adding 20 parts of wollastonite powder into 80 parts of PS, stirring for 10min by using a high-speed mixer, and then adding into a double-screw extruder for blending and extruding to obtain the wollastonite/PS composite material D5.
The PS composite materials prepared in the application example 5 and the comparative example 5 are made into sample strips by an injection molding machine, and the product performance data are shown in the following table:
as can be seen from the above table:
the tensile strength, bending strength and cantilever beam impact strength of X5 are higher than those of D5, which shows that the physical properties of PS modified by adding modified wollastonite powder are better than those of PS modified by adding only commercial wollastonite powder.
The technology describes a preparation method of modified wollastonite powder, and the prepared polyolefin material is improved in physical properties to a certain extent, so that the application field of the polyolefin composite material is greatly expanded, and the preparation method has very important significance.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (3)
1. A preparation method of modified wollastonite is characterized by comprising the following steps:
(1) weighing a certain amount of EVA emulsion, α -sulfo fatty acid methyl ester and deionized water, putting the mixture into a reaction vessel, reacting and stirring at normal temperature for 1-3h to obtain a solution A;
(2) weighing a certain amount of the solution A, wollastonite powder, calcium chloride and ethylene glycol monobutyl ether, putting the solution A, the wollastonite powder, the calcium chloride and the ethylene glycol monobutyl ether into a reaction vessel, reacting for 2-4h at 40-60 ℃, cooling, filtering and drying to obtain the modified wollastonite.
2. The method for preparing modified wollastonite of claim 1, wherein the mass ratio of the EVA emulsion, α -sulfo fatty acid methyl ester and the deionized water in the step (1) is (400-.
3. The method for preparing modified wollastonite according to claim 1, wherein the mass ratio of the solution A, the wollastonite powder, the calcium chloride and the ethylene glycol butyl ether in the step (2) is (20-30): (60-80): (1-3): (2-4).
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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 |
| 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 |
| 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 |
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| 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 |
| 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 |
| 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 |
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