CN108794707A - A kind of calcium carbonate powder of graft modification - Google Patents
A kind of calcium carbonate powder of graft modification Download PDFInfo
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- CN108794707A CN108794707A CN201810774678.3A CN201810774678A CN108794707A CN 108794707 A CN108794707 A CN 108794707A CN 201810774678 A CN201810774678 A CN 201810774678A CN 108794707 A CN108794707 A CN 108794707A
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- calcium carbonate
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- carbonate powder
- graft modification
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F292/00—Macromolecular compounds obtained by polymerising monomers on to inorganic materials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/08—Copolymers of ethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2451/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2451/10—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to inorganic materials
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- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
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Abstract
The invention belongs to calcium carbonate powder process for modifying surface fields, and in particular to a kind of calcium carbonate powder of graft modification.It is made by following steps：1）The preparation of modified acroleic acid；2）The preparation of ammonium persulfate aqueous solution；3）The preparation of modified poly ester lotion；4）The preparation of acid anhydrides dispersion liquid；5）The preparation of amide solution；6）The preparation of the calcium carbonate powder of graft modification.The calcium carbonate powder that the present invention is obtained by graft reaction improves the dispersion compatibility of calcium carbonate in the polymer.It in the modified poly ester lotion of the present invention, uses 2-mercaptobenzimidazole to handle acrylic monomers first, is then blended with ester monomer, polymerize under initiator effect, improve the antioxidant activity of polyester.The calcium carbonate powder of graft modification is applied in the preparation that LLDPE winds film by the present invention, improves the mechanical strength and stability of finished film.
Description
Technical field
The invention belongs to the modifies preparation fields of Paris white, and in particular to a kind of calcium carbonate powder of graft modification.
Background technology
Calcium carbonate is a kind of very common inorganic powdered filler, cheap, non-toxic and tasteless, whiteness is high, hardness is good
The advantages that, it is widely used in fields such as rubber product, papermaking, ink, plastics, coating.Winding film is mainly used for various
The sale and transport of product, main function is to consolidate, cover and protect product, so winding film must have higher wear well
Thorn property, good shrinkage and shrinkage stress.Initial winding film is continuous with requiring winding film properties based on PVC
It improves, PVC winding films gradually decrease, and various polyethylene winding film is quickly grown.
It is a kind of good material of toughness that polyethylene, which winds film, is widely used in drinks, pop can class, mineral water class, each
The one integral piece assembly package of the products such as kind of beverage class, cloth, the product flexibility is good, and impact resistance, tear resistance are strong, not cracky,
It is big tide, shrinking percentage are not afraid of.
However, winding film be easy to cause the uniform and stable property of finished films due to introducing inorganic filler calcium carbonate at present
Difference, influences quality of finished at phenomena such as being susceptible to blistering.
Invention content
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of Paris whites of graft modification
Body.
To achieve the above object, the present invention uses following technical scheme：
A kind of calcium carbonate powder of graft modification, is made by following steps：
（1）2-mercaptobenzimidazole is taken, is added in the chloroform of 10-13 times of its weight, stirs evenly, acrylic acid is added, is increased
Temperature is 50-55 DEG C, and insulated and stirred 1-2 hours is distilled off chloroform, obtains modified acroleic acid；
（2）Ammonium persulfate is taken, is added in the deionized water of 20-30 times of its weight, stirs evenly, obtain ammonium persulfate aqueous solution；
（3）Above-mentioned modified acroleic acid is taken, is blended with methyl acrylate, is stirred evenly, going for 10-14 times of mixture weight is added to
It in ionized water, stirs evenly, polypropylene glycerol aether is added, is sent in reaction kettle, be passed through nitrogen, adjusting temperature of reaction kettle is
65-70 DEG C, ammonium persulfate aqueous solution, insulated and stirred 4-5 hours is added, discharging cooling obtains modified poly ester lotion；
（4）Take precipitated calcium carbonate, maleic anhydride mixing that mixture weight 17- is added insulated and stirred 1-2 hours at 60-65 DEG C
It in 20 times of deionized water, stirs evenly, obtains acid anhydrides dispersion liquid；
（5）Divinylbenzene is taken, is added in the dimethylformamide of 3-5 times of its weight, stirs evenly, obtain amide solution；
（6）Above-mentioned modified poly ester lotion is taken, mixes, stirs evenly with acid anhydrides dispersion liquid, be sent in blender, above-mentioned acyl is added
Amine aqueous solution, at 65-79 DEG C, 1300-2000 revs/min stir 2-3 hour, discharging, suction filtration, filter cake is washed, 40-50 DEG C of vacuum
It lower dry 100-120 minutes, is cooled to room temperature, grinds, obtain the calcium carbonate powder of graft modification.
Preferably, the calcium carbonate powder of graft modification is applied to prepare LLDPE winding films by the present invention.
Preferably, the present invention mixes the calcium carbonate powder of graft modification, LLDPE, octyl mercaptan tin, plasticizer, stirring
Uniformly, it is sent in extruder, casting film-forming.
Preferably, modified poly ester lotion of the present invention is made of the raw material of following weight parts：
1-2 parts of 2-mercaptobenzimidazole, 20-30 parts of acrylic acid, 0.8-1 parts of ammonium persulfate, 20-30 parts of methyl acrylate, polyoxy
0.1-0.2 parts of propylene glycerin ether.
Preferably, step 4 of the present invention）To step 6）In, each raw material is counted in parts by weight, 1-2 parts of divinylbenzene, Malaysia
10-12 parts of acid anhydrides, 70-80 parts of modified poly ester lotion, 6-9 parts of precipitated calcium carbonate.
Preferably, each raw material of the present invention is counted in parts by weight, 8 parts of calcium carbonate powder, 130-140 parts of LLDPE, octyl sulphur
2-3 parts of alcohol tin, 10-14 parts of plasticizer.
Preferably, plasticizer of the present invention is one in tributyl citrate, triethyl citrate, epoxidized soybean oil
Kind.
The technological merit of the present invention：
（1）The calcium carbonate powder that the present invention is obtained by graft reaction improves the dispersion compatibility of calcium carbonate in the polymer.
（2）The present invention modified poly ester lotion in, first use 2-mercaptobenzimidazole handle acrylic monomers, then with
Ester monomer is blended, and polymerize under initiator effect, improves the antioxidant activity of polyester.
（3）The calcium carbonate powder of graft modification is applied in the preparation that LLDPE winds film by the present invention, improves finished film
Mechanical strength and stability.
（4）Each materials compatibility of winding film produced by the present invention is good, and the uniform and stable property of finished product is high, and profile pattern is good, nothing
Blistering, quality are high.
Specific implementation mode
The present invention is further described through with reference to embodiment.
Embodiment 1
（1）2 parts of 2-mercaptobenzimidazole is taken, is added in the chloroform of 13 times of its weight, stirs evenly, 30 parts of acrylic acid is added,
It is 55 DEG C to increase temperature, and insulated and stirred 2 hours is distilled off chloroform, obtains modified acroleic acid；
（2）1 part of ammonium persulfate is taken, is added in the deionized water of 30 times of its weight, is stirred evenly, obtain ammonium persulfate aqueous solution；
（3）Above-mentioned modified acroleic acid is taken, is blended for 30 parts, stirs evenly with methyl acrylate, be added to 14 times of mixture weight
It in deionized water, stirs evenly, 0.2 part of polypropylene glycerol aether is added, is sent in reaction kettle, be passed through nitrogen, adjust reaction
Kettle temperature degree is 70 DEG C, and ammonium persulfate aqueous solution, insulated and stirred 5 hours is added, and discharging cooling obtains modified poly ester lotion；
（4）12 parts of 9 parts of precipitated calcium carbonate, maleic anhydride mixing are taken, mixture weight is added in insulated and stirred 2 hours at 65 DEG C
It in 20 times of deionized water, stirs evenly, obtains acid anhydrides dispersion liquid；
（5）2 parts of divinylbenzene is taken, is added in the dimethylformamide of 5 times of its weight, is stirred evenly, obtain amide solution；
（6）80 parts of modified poly ester lotion is taken, mixes, stirs evenly with acid anhydrides dispersion liquid, be sent in blender, above-mentioned acyl is added
Amine aqueous solution, at 79 DEG C, 2000 revs/min stir 3 hours, discharge, filter, filter cake is washed, dry 100-120 at 50 DEG C of vacuum
Minute, it is cooled to room temperature, grinds, obtain the calcium carbonate powder of graft modification.
Embodiment 2
（1）1 part of 2-mercaptobenzimidazole is taken, is added in the chloroform of 10 times of its weight, stirs evenly, 20 parts of acrylic acid is added,
It is 50 DEG C to increase temperature, and insulated and stirred 1 hour is distilled off chloroform, obtains modified acroleic acid；
（2）0.8 part of ammonium persulfate is taken, is added in the deionized water of 20 times of its weight, is stirred evenly, it is water-soluble to obtain ammonium persulfate
Liquid；
（3）Above-mentioned modified acroleic acid is taken, is blended for 20 parts, stirs evenly with methyl acrylate, be added to 10 times of mixture weight
It in deionized water, stirs evenly, 0.1 part of polypropylene glycerol aether is added, is sent in reaction kettle, be passed through nitrogen, adjust reaction
Kettle temperature degree is 65 DEG C, and ammonium persulfate aqueous solution, insulated and stirred 4 hours is added, and discharging cooling obtains modified poly ester lotion；
（4）10 parts of 6 parts of precipitated calcium carbonate, maleic anhydride mixing are taken, mixture weight is added in insulated and stirred 1 hour at 60 DEG C
It in 17 times of deionized water, stirs evenly, obtains acid anhydrides dispersion liquid；
（5）1 part of divinylbenzene is taken, is added in the dimethylformamide of 3-5 times of its weight, stirs evenly, obtain amide solution；
（6）70 parts of above-mentioned modified poly ester lotion is taken, mixes, stirs evenly with acid anhydrides dispersion liquid, be sent in blender, in addition
State amide solution, at 65 DEG C, 1300 revs/min stir 2-3 hour, discharge, filter, filter cake is washed, at 40 DEG C of vacuum dry
It 100 minutes, is cooled to room temperature, grinds, obtain the calcium carbonate powder of graft modification.
Embodiment 3
8 parts of the calcium carbonate powder of graft modification in Example 1, with 140 parts of LLDPE, 3 parts of octyl mercaptan tin, citric acid three
14 parts of mixing of ethyl ester, stir evenly, are sent in extruder, and casting film-forming winds film to get acid anhydrides grafting LLDPE.
Embodiment 4
8 parts of the calcium carbonate powder of graft modification in Example 2, with 130 parts of LLDPE, 2 parts of octyl mercaptan tin, citric acid three
10 parts of mixing of butyl ester, stir evenly, are sent in extruder, and casting film-forming winds film to get acid anhydrides grafting LLDPE.
Acid anhydrides grafting LLDPE winding films made from embodiment 3 and 4 are tested for the property：
It is apparent it is smooth without blistering, without shrinkage cavity；
Fracture tensile strength：27-30MPa；
Elongation at break：330-405%；
Percent thermal shrinkage（130 DEG C × 20 seconds）MD：> 60.
Claims (7)
1. a kind of calcium carbonate powder of graft modification, it is characterised in that：It is made by following steps：
（1）2-mercaptobenzimidazole is taken, is added in the chloroform of 10-13 times of its weight, stirs evenly, acrylic acid is added, is increased
Temperature is 50-55 DEG C, and insulated and stirred 1-2 hours is distilled off chloroform, obtains modified acroleic acid；
（2）Ammonium persulfate is taken, is added in the deionized water of 20-30 times of its weight, stirs evenly, obtain ammonium persulfate aqueous solution；
（3）Above-mentioned modified acroleic acid is taken, is blended with methyl acrylate, is stirred evenly, going for 10-14 times of mixture weight is added to
It in ionized water, stirs evenly, polypropylene glycerol aether is added, is sent in reaction kettle, be passed through nitrogen, adjusting temperature of reaction kettle is
65-70 DEG C, ammonium persulfate aqueous solution, insulated and stirred 4-5 hours is added, discharging cooling obtains modified poly ester lotion；
（4）Take precipitated calcium carbonate, maleic anhydride mixing that mixture weight 17- is added insulated and stirred 1-2 hours at 60-65 DEG C
It in 20 times of deionized water, stirs evenly, obtains acid anhydrides dispersion liquid；
（5）Divinylbenzene is taken, is added in the dimethylformamide of 3-5 times of its weight, stirs evenly, obtain amide solution；
（6）Above-mentioned modified poly ester lotion is taken, mixes, stirs evenly with acid anhydrides dispersion liquid, be sent in blender, above-mentioned acyl is added
Amine aqueous solution, at 65-79 DEG C, 1300-2000 revs/min stir 2-3 hour, discharging, suction filtration, filter cake is washed, 40-50 DEG C of vacuum
It lower dry 100-120 minutes, is cooled to room temperature, grinds, obtain the calcium carbonate powder of graft modification.
2. a kind of calcium carbonate powder of graft modification according to claim 1, it is characterised in that：By the carbonic acid of graft modification
Calcium powder body is applied to prepare LLDPE winding films.
3. a kind of calcium carbonate powder of graft modification according to claim 2, it is characterised in that：By the carbonic acid of graft modification
Calcium powder body, LLDPE, octyl mercaptan tin, plasticizer mixing, stir evenly, are sent in extruder, casting film-forming.
4. a kind of calcium carbonate powder of graft modification according to claim 1, it is characterised in that：The modified poly ester breast
Liquid is made of the raw material of following weight parts：
1-2 parts of 2-mercaptobenzimidazole, 20-30 parts of acrylic acid, 0.8-1 parts of ammonium persulfate, 20-30 parts of methyl acrylate, polyoxy
0.1-0.2 parts of propylene glycerin ether.
5. a kind of calcium carbonate powder of graft modification according to claim 1, it is characterised in that：Step 4）To step 6）
In, each raw material is counted in parts by weight, 1-2 parts of divinylbenzene, 10-12 parts of maleic anhydride, 70-80 parts of modified poly ester lotion, light
6-9 parts of matter calcium carbonate.
6. a kind of calcium carbonate powder of graft modification according to claim 3, it is characterised in that：Each raw material is by weight
Number meter, 8 parts of calcium carbonate powder, 130-140 parts of LLDPE, 2-3 parts of octyl mercaptan tin, 10-14 parts of plasticizer.
7. a kind of calcium carbonate powder of graft modification according to claim 6, it is characterised in that：The plasticizer is lemon
One kind in lemon acid tributyl, triethyl citrate, epoxidized soybean oil.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810774678.3A CN108794707A (en) | 2018-07-16 | 2018-07-16 | A kind of calcium carbonate powder of graft modification |
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| CN201810774678.3A CN108794707A (en) | 2018-07-16 | 2018-07-16 | A kind of calcium carbonate powder of graft modification |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1539861A (en) * | 2003-10-29 | 2004-10-27 | 中山大学 | Method for modifying inorganic particles through grafting in situ by ball milling method |
| CN103539976A (en) * | 2013-10-29 | 2014-01-29 | 中国热带农业科学院农产品加工研究所 | Preparation method of reinforced natural rubber composite material by grafting hydroxyethyl methacrylate rubber with modified nano calcium carbonate |
| CN106590042A (en) * | 2016-10-20 | 2017-04-26 | 青阳县永诚钙业有限责任公司 | Calcium carbonate powder modified by grafting of self dispersible polymer-maleic anhydride and preparation method thereof |
-
2018
- 2018-07-16 CN CN201810774678.3A patent/CN108794707A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1539861A (en) * | 2003-10-29 | 2004-10-27 | 中山大学 | Method for modifying inorganic particles through grafting in situ by ball milling method |
| CN103539976A (en) * | 2013-10-29 | 2014-01-29 | 中国热带农业科学院农产品加工研究所 | Preparation method of reinforced natural rubber composite material by grafting hydroxyethyl methacrylate rubber with modified nano calcium carbonate |
| CN106590042A (en) * | 2016-10-20 | 2017-04-26 | 青阳县永诚钙业有限责任公司 | Calcium carbonate powder modified by grafting of self dispersible polymer-maleic anhydride and preparation method thereof |
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Application publication date: 20181113 |