CN110452558A - Method for preparing nano calcium carbonate for hard PVC - Google Patents
Method for preparing nano calcium carbonate for hard PVC Download PDFInfo
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- CN110452558A CN110452558A CN201910800514.8A CN201910800514A CN110452558A CN 110452558 A CN110452558 A CN 110452558A CN 201910800514 A CN201910800514 A CN 201910800514A CN 110452558 A CN110452558 A CN 110452558A
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- CN
- China
- Prior art keywords
- calcium carbonate
- hard pvc
- nano calcium
- nanometer calcium
- preparing
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title claims abstract description 163
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 82
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000000725 suspension Substances 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 239000004698 Polyethylene Substances 0.000 claims abstract description 20
- 239000004593 Epoxy Substances 0.000 claims abstract description 19
- -1 polyethylene Polymers 0.000 claims abstract description 19
- 229920000573 polyethylene Polymers 0.000 claims abstract description 19
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 claims abstract description 18
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000811 xylitol Substances 0.000 claims abstract description 18
- 235000010447 xylitol Nutrition 0.000 claims abstract description 18
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 claims abstract description 18
- 229960002675 xylitol Drugs 0.000 claims abstract description 18
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims abstract description 12
- 235000011941 Tilia x europaea Nutrition 0.000 claims abstract description 12
- 239000004571 lime Substances 0.000 claims abstract description 12
- 235000013336 milk Nutrition 0.000 claims abstract description 12
- 239000008267 milk Substances 0.000 claims abstract description 12
- 210000004080 milk Anatomy 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- 230000018044 dehydration Effects 0.000 claims abstract description 10
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 18
- 235000019486 Sunflower oil Nutrition 0.000 claims description 17
- 239000002600 sunflower oil Substances 0.000 claims description 17
- 239000000920 calcium hydroxide Substances 0.000 claims description 8
- 235000011116 calcium hydroxide Nutrition 0.000 claims description 8
- 238000013329 compounding Methods 0.000 claims description 8
- 238000004381 surface treatment Methods 0.000 claims description 3
- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 claims 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 1
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 claims 1
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 claims 1
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 9
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 6
- 230000004048 modification Effects 0.000 abstract description 3
- 238000012986 modification Methods 0.000 abstract description 3
- 239000001569 carbon dioxide Substances 0.000 abstract description 2
- 230000005484 gravity Effects 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 235000019198 oils Nutrition 0.000 abstract description 2
- 238000003825 pressing Methods 0.000 abstract description 2
- 235000020238 sunflower seed Nutrition 0.000 abstract description 2
- 230000005587 bubbling Effects 0.000 abstract 1
- 239000012756 surface treatment agent Substances 0.000 abstract 1
- 235000010216 calcium carbonate Nutrition 0.000 description 66
- 239000004800 polyvinyl chloride Substances 0.000 description 54
- 229920000915 polyvinyl chloride Polymers 0.000 description 54
- 239000000047 product Substances 0.000 description 9
- 238000004364 calculation method Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 239000002131 composite material Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 239000004094 surface-active agent Substances 0.000 description 5
- 241000276489 Merlangius merlangus Species 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 229920003023 plastic Polymers 0.000 description 4
- 239000004033 plastic Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 230000005764 inhibitory process Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 230000003014 reinforcing effect Effects 0.000 description 3
- 206010023126 Jaundice Diseases 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- IHBCFWWEZXPPLG-UHFFFAOYSA-N [Ca].[Zn] Chemical compound [Ca].[Zn] IHBCFWWEZXPPLG-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 238000001994 activation Methods 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 239000012760 heat stabilizer Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000011265 semifinished product Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
Classifications
-
- 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
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/02—Compounds of alkaline earth metals or magnesium
- C09C1/021—Calcium carbonates
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
-
- 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
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a method for preparing nano calcium carbonate for hard PVC, which comprises the steps of adjusting the specific gravity of refined lime milk to 1.060 ~ 1.070.070, introducing into a bubbling carbonation reaction kettle, adjusting the temperature of the lime milk to 25 ~ 30 ℃, introducing mixed gas containing carbon dioxide to carry out carbonation reaction until the pH value is =7.0, heating nano calcium carbonate suspension to 75 ~ 90 ℃, adding a surface treatment agent compounded by carboxylated polyethylene wax, epoxy sunflower seed oil and xylitol, stirring for 30-60min to complete surface modification, carrying out filter pressing, dehydration, drying and crushing on the nano calcium carbonate suspension subjected to surface modification to obtain the nano calcium carbonate for hard PVC.
Description
Technical field
The present invention relates to nano-material modified technical field, specifically a kind of side for preparing hard PVC nanometer calcium carbonate
Method.
Background technique
Hard PVC composite material is usually to be made of polyvinyl chloride resin, filler and auxiliary agent, and be widely used in chemical industry, building materials
Equal fields.But PVC composite material is in process, polyvinyl chloride resin generates hair vulnerable to thermal decomposition, so as to cause PVC product
The form and aspect problems such as red, jaundice.
For nanometer calcium carbonate since its reinforcing property is good, loading is big, cheap, and having in hard PVC filling can not
The advantage of analogy.But during the processing plasticizing of PVC, since nanometer calcium carbonate partial size is small, coefficient of friction is big, be easy by
Friction causes processing temperature is excessively high PVC is caused to thermally decompose, to lead to the problem of form and aspect, limits its application range.
In conclusion there is larger in terms of the form and aspect of PVC product when existing nanometer calcium carbonate is as hard PVC filler
Limitation, it is therefore, necessary to the further investigation of filler.
Patent CN 106832660A discloses a kind of method that rod-like precipitates calcium carbonate improves hard PVC profile performance, with
Shock resistance hard PVC profile, product raw material and parts by weight are made in the calcium carbonate-filled PVC of rod-like precipitates are as follows: PVC-
SG5100.0 parts；5.0-60.0 parts of rod-like precipitates calcium carbonate；4.0-12.0 parts of calcium-zinc composite stabilizing agent；0.4-1.3 parts of stearic acid；
0.2-1.0 parts of PE wax；0.5-1.2 parts of titanium dioxide；1.0-5.5 parts of ACR-401.The hard PVC profile of this method preparation has excellent
Erosion-resisting characteristics and tensile strength, CaCO3 and when PVC mixing ratio 40/100, notch impact strength is increased to from 6.3KJ/m2
9.5KJ/m2, tensile strength are increased to 39.7MPa from 33.1MPa, and elongation at break is increased to 11.4% from 6.7%, and highest is mixed
Composition and division in a proportion substantially reduces the production cost of hard PVC profile up to 60/100, and profile has lower counter balance torque and higher
Rate of extrusion, processing fluidity are preferable.The patent has studied calcium carbonate to the reinforcing property of hard PVC, without to hard emphatically
The form and aspect problem of matter PVC is studied.
Patent CN 106833026A discloses a kind of PVC powdered whiting surface treatment method, is that will compare table after ink
Reaction kettle heating is added in the powdered whiting that area is 3-8m2/g, and temperature is controlled at 50-90 DEG C, and acrylic emulsion, stirring is added
10-30min completes the first subsurface and is modified, and ammonium sulfate and ten is added in the modified obtained powdered whiting of the first subsurface
Dialkyl group mercaptan stirs 30-60min, and the surface for completing powdered whiting is modified, and dehydration and drying obtains the product.This method
The calcium carbonate of preparation has good dispersibility and reinforcing property, but the research object is not nanometer calcium carbonate, and is not had
Form and aspect are studied.
Patent CN 107915933A discloses a kind of preparation method of dedicated toughened nano calcium carbonate of PVC plastic, by stone
Ash is mixed with tap water carries out digestion reaction, obtains refined lime milk solution by screening out miscellaneous, standing；By lime milk solution specific gravity
It adjusts to 1.050-1.070, it is cooling, it is delivered to the carbonization kettle with stirring, and be passed through purified kiln gas and carry out carbonation reaction,
Until reaction system pH < 7.3, carbonation reaction is completed to arrive nanometer calcium carbonate slurries；Slurries are heated to, and add fat
Acid sodium-salt carries out surface activation process, and filters pressing obtains filter cake；Filtration cakes torrefaction crushes, and nanometer calcium carbonate semi-finished product are made；It is last defeated
It send to continuing modifier, adds acrylamide-styrene copolymer and haloflex carries out surface and is modified, i.e., toughening type is received
Rice calcium carbonate product.The nanometer calcium carbonate of invention preparation has good processability and dispersibility, can significantly improve PVC plastic
The intensity and impact resistance of material, the invention do not study the form and aspect of hard PVC.
The disclosure of background above technology contents is only used for auxiliary and understands inventive concept and technical solution of the invention, not
The prior art for necessarily belonging to present patent application shows above content in the applying date of present patent application in no tangible proof
In the case where having disclosed, above-mentioned background technique should not be taken to the novelty and creativeness of evaluation the application.
Summary of the invention
The present invention it is existing it is nono calcium carbonate modified there are aiming at the problem that, provide and a kind of prepare hard PVC nano-calcium carbonate
The method of calcium.The modified obtained nanometer calcium carbonate of this method is not only able to satisfy the toughening demand of hard PVC, moreover it is possible to improve hard
The flavescence of PVC, the problems such as reddening.
The present invention is realized based on following principle:
Selected nanometer calcium carbonate surface treating agent is answered by the polyethylene wax, epoxy sunflower oil and xylitol of carboxylated
It is modified to nanometer calcium carbonate progress surface to close formula.PVC can be effectively reduced due to its lubricating action in the polyethylene wax of carboxylated
Frictional heat generation amount in process.The Cl in PVC decomposable process then can be absorbed in epoxy sunflower oil, reaches inhibition and decomposes
Effect.Xylitol then does secondary heat stabilizer effect.So as to make PVC achieve the effect that color inhibition.
This hair is achieved through the following technical solutions:
A method of hard PVC nanometer calcium carbonate is prepared, is included the following steps:
(1) refined lime milk density is adjusted to 1.060~1.070, then introduces and is bubbled carbonation reaction kettle, milk of lime temperature
Degree is adjusted to 25~30 DEG C, is passed through the mixed gas containing carbon dioxide and carries out carbonation reaction to pH=7.0, obtains nanometer calcium carbonate
Suspension；
(2) nano calcium carbonate suspension is heated to 75~90 DEG C, polyethylene wax, epoxy sunflower seeds by carboxylated is added
Surface treating agent made of oil and xylitol compounding, after stirring 30-60min, it is modified to complete surface；
(3) the modified nano calcium carbonate suspension in surface will be completed and passes through filter-press dehydration, dry, pulverize, can be obtained hard
Matter PVC nanometer calcium carbonate.
Preferably, the usage amount of the surface treating agent is the 2.0~3.0% of calcium carbonate butt quality.
Preferably, the polyethylene wax inorganic agent quality of carboxylated accounts for the 30 of surface treating agent total amount in the surface treating agent
The 55~65% of the total treatment dosage of~40%, epoxy sunflower oil Zhan, the 5% of the total finish level of xylitol Zhan.
Preferably, the carbonation reaction is the mixed gas for being passed through CO2 concentration and being 33%.
Preferably, the drying is to be placed in drying in 100~110 DEG C of baking ovens.
Compared with prior art, it advantages of the present invention and has the beneficial effect that
1, the present invention is by being added the surface as made of polyethylene wax, epoxy sunflower oil and the xylitol compounding of carboxylated
It is modified that inorganic agent carries out surface to nanometer calcium carbonate so that product obtained have lower moisture absorption, excellent processing performance,
The performances such as mechanical property, color inhibition.
2, after nanon calcium carbonatefilled hard PVC produced by the present invention, the toughening need of filling hard PVC can not only be met
It asks, moreover it is possible to the form and aspect problem such as improve the flavescence of hard PVC, redden.
3, present invention process simple possible, production cost is low, has preferable economic benefit and social benefit, easy to accomplish
Industrialized production.
Specific embodiment
The present invention program is further described below in conjunction with specific embodiment, but is not limited to protection model of the invention
It encloses.
Embodiment 1
A method of hard PVC nanometer calcium carbonate is prepared, is included the following steps:
(1) refined lime milk density is adjusted to 1.065, then introduces and is bubbled carbonation reaction kettle, milk of lime temperature is adjusted to
25 DEG C, it is passed through CO2The mixed gas that concentration is 33% carries out carbonation reaction to pH=7.0, obtains nano calcium carbonate suspension；
(2) nano calcium carbonate suspension is heated to 80 DEG C, with calcium carbonate dry base Mass Calculation with 2.5% amount be added by
Surface treating agent made of the polyethylene wax of carboxylated, epoxy sunflower oil and xylitol compounding, carboxylic in the surfactant
The mass percent that polyethylene wax, epoxy sunflower oil and the xylitol of base respectively account for is respectively 35%, 60%, 5%, stirring
After 40min, it is modified to complete surface；
(3) the modified nano calcium carbonate suspension in surface will be completed and passes through filter-press dehydration, and be placed in drying in 100 DEG C of baking ovens,
It crushes, hard PVC nanometer calcium carbonate can be obtained.
Embodiment 2
A method of hard PVC nanometer calcium carbonate is prepared, is included the following steps:
(1) refined lime milk density is adjusted to 1.070, then introduces and is bubbled carbonation reaction kettle, milk of lime temperature is adjusted to
28 DEG C, it is passed through CO2The mixed gas that concentration is 33% carries out carbonation reaction to pH=7.0, obtains nano calcium carbonate suspension；
(2) nano calcium carbonate suspension is heated to 75 DEG C, with calcium carbonate dry base Mass Calculation with 3.0% amount be added by
Surface treating agent made of the polyethylene wax of carboxylated, epoxy sunflower oil and xylitol compounding, carboxylic in the surfactant
The mass percent that polyethylene wax, epoxy sunflower oil and the xylitol of base respectively account for is respectively 40%, 55%, 5%, stirring
After 40min, it is modified to complete surface；
(3) the modified nano calcium carbonate suspension in surface will be completed and passes through filter-press dehydration, and be placed in drying in 105 DEG C of baking ovens,
It crushes, hard PVC nanometer calcium carbonate can be obtained.
Embodiment 3
A method of hard PVC nanometer calcium carbonate is prepared, is included the following steps:
(3) refined lime milk density is adjusted to 1.060, then introduces and is bubbled carbonation reaction kettle, milk of lime temperature is adjusted to
30 DEG C, it is passed through CO2The mixed gas that concentration is 33% carries out carbonation reaction to pH=7.0, obtains nano calcium carbonate suspension；
(4) nano calcium carbonate suspension is heated to 85 DEG C, with calcium carbonate dry base Mass Calculation with 2.0% amount be added by
Surface treating agent made of the polyethylene wax of carboxylated, epoxy sunflower oil and xylitol compounding, carboxylic in the surfactant
The mass percent that polyethylene wax, epoxy sunflower oil and the xylitol of base respectively account for is respectively 35%, 60%, 5%, stirring
After 45min, it is modified to complete surface；
(3) the modified nano calcium carbonate suspension in surface will be completed and passes through filter-press dehydration, and be placed in drying in 110 DEG C of baking ovens,
It crushes, hard PVC nanometer calcium carbonate can be obtained.
Embodiment 4
A method of hard PVC nanometer calcium carbonate is prepared, is included the following steps:
(1) refined lime milk density is adjusted to 1.065, then introduces and is bubbled carbonation reaction kettle, milk of lime temperature is adjusted to
25 DEG C, it is passed through CO2The mixed gas that concentration is 33% carries out carbonation reaction to pH=7.0, obtains nano calcium carbonate suspension；
(2) nano calcium carbonate suspension is heated to 85 DEG C, with calcium carbonate dry base Mass Calculation with 3.0% amount be added by
Surface treating agent made of the polyethylene wax of carboxylated, epoxy sunflower oil and xylitol compounding, carboxylic in the surfactant
The mass percent that polyethylene wax, epoxy sunflower oil and the xylitol of base respectively account for is respectively 35%, 60%, 5%, stirring
After 60min, it is modified to complete surface；
(3) the modified nano calcium carbonate suspension in surface will be completed and passes through filter-press dehydration, and be placed in drying in 110 DEG C of baking ovens,
It crushes, hard PVC nanometer calcium carbonate can be obtained.
Embodiment 5
A method of hard PVC nanometer calcium carbonate is prepared, is included the following steps:
(1) refined lime milk density is adjusted to 1.070, then introduces and is bubbled carbonation reaction kettle, milk of lime temperature is adjusted to
26 DEG C, it is passed through CO2The mixed gas that concentration is 33% carries out carbonation reaction to pH=7.0, obtains nano calcium carbonate suspension；
(2) nano calcium carbonate suspension is heated to 80 DEG C, with calcium carbonate dry base Mass Calculation with 2.5% amount be added by
Surface treating agent made of the polyethylene wax of carboxylated, epoxy sunflower oil and xylitol compounding, carboxylic in the surfactant
The mass percent that polyethylene wax, epoxy sunflower oil and the xylitol of base respectively account for is respectively 40%, 55%, 5%, stirring
After 40min, it is modified to complete surface；
(3) the modified nano calcium carbonate suspension in surface will be completed and passes through filter-press dehydration, and be placed in drying in 110 DEG C of baking ovens,
It crushes, hard PVC nanometer calcium carbonate can be obtained.
Comparative example
(1) refined lime milk density is adjusted to 1.070, then introduces and is bubbled carbonation reaction kettle, milk of lime temperature is adjusted to
26 DEG C, it is passed through CO2The mixed gas that concentration is 33% carries out carbonation reaction to pH=7.0, obtains nano calcium carbonate suspension；
(2) nano calcium carbonate suspension is heated to 80 DEG C, is added firmly with calcium carbonate dry base Mass Calculation with 2.5% amount
After stirring 40min, it is modified to complete surface for matter acid sodium；
(3) the modified nano calcium carbonate suspension in surface will be completed and passes through filter-press dehydration, and be placed in drying in 110 DEG C of baking ovens,
It crushes, hard PVC nanometer calcium carbonate can be obtained.
Nanon calcium carbonatefilled hard PVC produced by the present invention
1-5 of the embodiment of the present invention and the comparative example nanometer calcium carbonate prepared are pressed in table 1 by formula in high-speed mixer
In be kneaded 20min in advance, be granulated and be molded through double screw extruder and injection molding machine respectively, obtain PVC plastic test sample.
Table 1: hard PVC composite-material formula
Properties of product test is carried out to above-mentioned PVC plastic test sample, GB/T1040.2- is pressed in wherein tensile strength test
Method as defined in 2006 carries out；Impact strength is carried out by method as defined in GB/T 1043.1-2006, with the auspicious instrument instrument of Shanghai sunrise
The La*b* value of the WSB-3A leucometer measurement test sample of table Co., Ltd, test result are as shown in table 2.
Table 2:PVC composite property test result
It is learnt from the data of table 2, WI value (Hunter whiteness), the b* value of comparative example all have huge difference with embodiment
Not, illustrate the product of comparative example much than embodiment sample Huang, on the one hand due to the lubricant effect of stearate, much than not
The polyethylene wax of upper carboxylated, friction cause processing temperature to cross high PVC decomposition, are on the other hand due to not having epoxy sunflower oil
PVC decomposition is inhibited with xylitol.In terms of reinforcement, embodiment also shows preferable effect, illustrates of the invention real
Apply the modified obtained nanometer calcium carbonate and the more preferable reason of PVC compatibility of example.Therefore, nanometer calcium carbonate prepared by the present invention produces
Product not only can satisfy filling hard PVC to the conventional requirement of toughening, can also be effectively improved hard PVC jaundice problem, market
Application prospect is very extensive.
The above content is combine it is specific/further detailed description of the invention for preferred embodiment, cannot
Assert that specific implementation of the invention is only limited to these instructions.General technical staff of the technical field of the invention is come
It says, without departing from the inventive concept of the premise, some replacements or modifications can also be made to the embodiment that these have been described,
And these substitutions or variant are regarded as belonging to the scope of protection of the present invention.
Claims (5)
1. a kind of method for preparing hard PVC nanometer calcium carbonate, characterized by the following steps:
Refined lime milk density is adjusted to 1.060 ~ 1.070, then introduces and is bubbled carbonation reaction kettle, milk of lime temperature is adjusted to 25
It ~ 30 DEG C, is passed through carbonated mixed gas and carries out carbonation reaction to pH=7.0, obtain nano calcium carbonate suspension；
Nano calcium carbonate suspension is heated to 75 ~ 90 DEG C, polyethylene wax, epoxy sunflower oil and xylose by carboxylated is added
After stirring 30-60min, it is modified to complete surface for surface treating agent made of alcohol compounding；
It will complete the modified nano calcium carbonate suspension in surface and pass through filter-press dehydration, dry, pulverize, hard PVC use can be obtained
Nanometer calcium carbonate.
2. preparing the method for hard PVC nanometer calcium carbonate according to claim 1, it is characterised in that: the surface treatment
The usage amount of agent is the 2.0 ~ 3.0% of calcium carbonate butt quality.
3. preparing the method for hard PVC nanometer calcium carbonate according to claim 2, it is characterised in that: the surface treatment
The polyethylene wax inorganic agent quality of carboxylated accounts for the 30 ~ 40% of surface treating agent total amount in agent, the total inorganic agent of epoxy sunflower oil Zhan
The 55 ~ 65% of amount, the 5% of the total finish level of xylitol Zhan.
4. preparing the method for hard PVC nanometer calcium carbonate according to claim 1, it is characterised in that: the carbonating is anti-
It should be and be passed through the mixed gas that CO2 concentration is 33%.
5. preparing the method for hard PVC nanometer calcium carbonate according to claim 1, it is characterised in that: the drying is to set
It is dry in 100 ~ 110 DEG C of baking ovens.
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| CN112960685A (en) * | 2021-03-04 | 2021-06-15 | 安徽省宣城市华纳新材料科技有限公司 | Preparation method of nano calcium carbonate for filling hard PVC (polyvinyl chloride) |
| CN114316631A (en) * | 2021-12-28 | 2022-04-12 | 广西华纳新材料科技有限公司 | Functionalized nano calcium carbonate for hard PVC |
| CN116789157A (en) * | 2023-05-19 | 2023-09-22 | 广西华纳新材料股份有限公司 | Preparation method of nano calcium carbonate for automobile welding seam sealant |
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