CN1004076B - Process for preparation of beta-crystalline polypropylene - Google Patents
Process for preparation of beta-crystalline polypropylene Download PDFInfo
- Publication number
- CN1004076B CN1004076B CN85100465.2A CN85100465A CN1004076B CN 1004076 B CN1004076 B CN 1004076B CN 85100465 A CN85100465 A CN 85100465A CN 1004076 B CN1004076 B CN 1004076B
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- China
- Prior art keywords
- beta
- component
- polypropylene
- crystalline
- production method
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000004743 Polypropylene Substances 0.000 title claims abstract description 29
- -1 polypropylene Polymers 0.000 title claims abstract description 29
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title description 7
- 238000002360 preparation method Methods 0.000 title description 2
- 238000004519 manufacturing process Methods 0.000 claims abstract description 14
- 239000002253 acid Substances 0.000 claims abstract description 5
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims abstract 3
- 150000001342 alkaline earth metals Chemical class 0.000 claims abstract 3
- 239000002667 nucleating agent Substances 0.000 claims abstract 3
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 claims description 4
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 2
- 239000000292 calcium oxide Substances 0.000 claims description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims 1
- 150000001341 alkaline earth metal compounds Chemical class 0.000 claims 1
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 claims 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims 1
- 239000000395 magnesium oxide Substances 0.000 claims 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims 1
- 125000000896 monocarboxylic acid group Chemical group 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 abstract description 6
- 238000002156 mixing Methods 0.000 abstract description 5
- 239000000047 product Substances 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 3
- 239000000835 fiber Substances 0.000 abstract description 2
- 230000003179 granulation Effects 0.000 abstract description 2
- 238000010128 melt processing Methods 0.000 abstract description 2
- 239000000470 constituent Substances 0.000 abstract 1
- 238000007909 melt granulation Methods 0.000 abstract 1
- 230000000737 periodic effect Effects 0.000 abstract 1
- 239000010409 thin film Substances 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 17
- BKIMMITUMNQMOS-UHFFFAOYSA-N nonane Chemical compound CCCCCCCCC BKIMMITUMNQMOS-UHFFFAOYSA-N 0.000 description 8
- 238000002425 crystallisation Methods 0.000 description 6
- 230000008025 crystallization Effects 0.000 description 6
- 239000012982 microporous membrane Substances 0.000 description 4
- WLJVNTCWHIRURA-UHFFFAOYSA-N pimelic acid Chemical compound OC(=O)CCCCCC(O)=O WLJVNTCWHIRURA-UHFFFAOYSA-N 0.000 description 4
- 239000004925 Acrylic resin Substances 0.000 description 3
- 229920000178 Acrylic resin Polymers 0.000 description 3
- 239000004594 Masterbatch (MB) Substances 0.000 description 3
- NRCMAYZCPIVABH-UHFFFAOYSA-N Quinacridone Chemical compound N1C2=CC=CC=C2C(=O)C2=C1C=C1C(=O)C3=CC=CC=C3NC1=C2 NRCMAYZCPIVABH-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 239000002932 luster Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 150000007522 mineralic acids Chemical class 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 241000276489 Merlangius merlangus Species 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920005676 ethylene-propylene block copolymer Polymers 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 238000009998 heat setting Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 229920005629 polypropylene homopolymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 238000000108 ultra-filtration Methods 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
-
- 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
- C08K3/10—Metal compounds
- C08K3/105—Compounds containing metals of Groups 1 to 3 or of Groups 11 to 13 of the Periodic Table
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Extrusion Moulding Of Plastics Or The Like (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
The present invention belongs to beta-crystalline polypropylene, a production method thereof and the application thereof. The content of the beta-crystalline polypropylene is from 80 to 93%. The beta-crystalline polypropylene is produced by mixing a double-constituent beta-crystalline nucleating agent and polypropylene through melt processing and granulation, wherein the nucleating agent is prepared from 1*10<-2> to 1 wt% of organic dibasic acid and 0.2 to 1 wt% of compounds of alkaline earth metal in the second group of a periodic table. The beta-crystalline polypropylene is a material for manufacturing high impact resistance products, thin films, fibers, etc. 33:02).
Description
The invention relates to the beta-crystal polypropylene production method.
The common multiple crystal formation of the crystallizable one-tenth of polypropylene, α or monoclinic form are the most stable and modal a kind of, and the polypropylene content of β or hexagonal structure is very few.
The relative content of beta crystal in polypropylene is to record with X-ray diffraction method, can calculate from following formula:
K=H
300/H
300+H
040+H
110+H
130
K represents the relative content of beta crystal in polypropylene, H in the formula
300Be the height of the strongest beta crystal (300) diffraction peak, H
040, H
110, H
130Be three diffraction peaks the strongest (040) of alpha-crystal form, (110), the height of (130), when not containing beta crystal in the sample, K=0.
In order to obtain to have the polypropylene of higher beta-crystalline form content, need in the production method of preparation Beta-crystalline polyacrylic, add the compound that plays the nucleus effect on a small quantity, this compound is called beta crystal-type nucleater.Being acknowledged as the most effective nucleator at present is quinacridine (quinacridone), i.e. dyestuff permanent red E3B.But under general condition, the beta-crystalline form content that this nucleator exists crystallization down to obtain is lower than 60%, (W.Ullmann and J.H.Wendorfy, Progr.Colloid Polymer Sci., 66,25-33(1979)).Reported that individually beta-crystalline form content can reach 85%(P.Forgacs, B.F.Tolochka and M.A.Sheromov, Polymer Bulletin, 6,127-133(1981)).Making the Beta-crystalline polyacrylic that nucleator will obtain up to 85% content with dyestuff permanent red E3B is the comparison difficulty, and the Beta-crystalline polyacrylic product that obtains has color, and poor heat stability changes into alpha-crystal form easily.The Japan clear 57-172943 of special permission communique has reported the quinacridine compounds has been added in the catalyst for polymerization of propylene, melt extrudes after the polymerization, and crystallization under 10 ℃/minute speed of cooling, recording its beta-crystalline form content with the DSC method is 63-88%.Because the DSC method is not to measure the standard method of beta-crystalline form content, and this method requirement polypropylene crystallization under 10 ℃ of/minute slow refrigerative conditions, differing greatly with actual production conditions, limitation is very big.Therefore, the beta-crystalline form content that this special permission communique is reported is suspectable, and this product takes on a red color poor stability.
The purpose of this invention is to provide a kind of beta-crystalline form content height, the polypropylene of good stability also provides the Beta-crystalline polyacrylic production method of two-pack compound as beta crystal-type nucleater simultaneously.In the presence of this nucleator, can under general condition obtain the polypropylene of beta-crystalline form content.The object of the invention also comprises the goods that the Beta-crystalline polyacrylic with higher shock strength is provided and prepares microporous membrane etc. from Beta-crystalline polyacrylic.
Beta-crystalline polyacrylic provided by the invention, the content that records its beta crystal with X-ray diffraction method is up to 93%, and promptly the K value is 0.93, and between 85-93%, this Beta-crystalline polyacrylic is nontoxic usually, and its outward appearance and color and luster are identical with raw material.
The production method of Beta-crystalline polyacrylic provided by the invention is with polypropylene and the pre-mixing by a certain percentage of two-pack beta crystal-type nucleater, mixes in molten state again, make then its in the presence of nucleator from the molten state crystallization.Melt processing temperature generally is controlled at 200~220 ℃ between 180-300 ℃, with the molecular weight of acrylic resin or melting index and different, also relevant with processing molding method.The melting mixing of polypropylene and nucleator can be finished in single screw extrusion machine, can adopt the commodity granular resin to make raw material.
Beta crystal-type nucleater provided by the invention is to be mixed by component A and B component.Component A is an organic dibasic acid, as pimelic acid, and nonane diacid, adjacent, to the phthalic acid of a, position.B component is an II in the periodictable
AThe oxide compound of family's metallic element, oxyhydroxide, the salt of organic and inorganic acid, this metallic element can be magnesium, calcium, strontium, barium.The salt of organic and inorganic acid can be the salt of stearic acid, carbonic acid.The consumption of component A is in 0.0001-5%(weight) scope, it recommends consumption is 0.01-1%(weight), the consumption of B component is a 0.001-5%(weight) scope, it recommends consumption is 0.05-1%(weight), A and B are added in the acrylic resin and get final product during use.
Can make various polypropylene articles with Beta-crystalline polyacrylic of the present invention, Beta-crystalline polyacrylic stretches when changing into alpha-crystal form, produces micropore simultaneously, can make microporous membrane, and various polypropylene articles comprise:
1. high-impact goods, it can be an injecting products, tubing, sheet material or bar, the polypropylene content of the beta crystal of these goods>85%.
2. film, it can be the alligatoring film that the electric power container is used, and can print the microporous membrane that the film write and ultrafiltration are used.
3. fiber, silk and rope etc.Have soft, chromatophilous advantage.
Beta-crystalline polyacrylic of the present invention is nontoxic, and its outward appearance and color and luster are identical with material resin, and has the thermostability height, and permanent the placement can not changed alpha-crystal form into yet under melt temperature.Even cooling off slowly or soon or crystallization under comparatively high temps when melt-processed, the product that obtains has ductility not rupture in not embrittlement of room temperature during stretching, and general acrylic resin is easy to fracture under these conditions.The Beta-crystalline polyacrylic that the present invention makes mechanical property at room temperature all is better than alpha-crystal form, and its numerical value is listed in table 1 and the table 2.
Table 1. α and Beta-crystalline polyacrylic are 23 ℃ mechanical property
The polypropylene of table 2. α and beta crystal is 23 ℃ breach shock strength
From table 1, table 2 as can be known, the alpha-crystal form of the Beta-crystalline polyacrylic and the same trade mark relatively has higher shock strength, lower yield strength.
Example 1
With 100 parts of particulate state homopolymer polypropylenes, 0.1 part of nonane diacid, 0.1 part of whiting, behind the uniform mixing, heating is extruded then through melting mixing in single screw extrusion machine, and cooling granulation just obtains the Beta-crystalline polyacrylic master batch.This master batch can mainly be contained the polypropylene of beta crystal after melt-processed, its content is variant slightly with crystallization condition, and the K value is 0.85~0.93.
Example 2
Replace nonane diacid with pimelic acid, condition such as example 1, the Beta-crystalline polyacrylic content that obtains (in the K value) is>0.90.
Example 3
Make nucleator with 0.1 part of terephthalic acid and 0.1 part of calcium oxide and replace beta nucleater in the example 1, repeat example 1, the Beta-crystalline polyacrylic content that obtains (in the K value) 0.85.
Example 4
Replace the homo-polypropylene in the example 1 to repeat example 1 with Ethylene-Propylene Block Copolymer, the Beta-crystalline polyacrylic content that obtains (in the K value) is 0.85~0.93.
Example 5
With 0.1 part of nonane diacid, 0.1 part of barium oxide is done the experiment that nucleator repeats example 1, and the Beta-crystalline polyacrylic content that obtains (in the K value) is 0.70~0.93.
Example 6
The beta-crystal polypropylene master batch that use-case 1 makes is extruded the form flat film postcooling with flat film machine, again at 60~150 ℃, and unidirectional or two-way stretch.Behind the drawn, this flat film is transformed into milky microporous membrane, and density descends, and carries out heat setting type then, stablizes its pore structure.The film that makes like this, its whiteness are 95%, and available oiliness ink printing is write.
Claims (6)
1, a kind of Beta-crystalline polyacrylic production method that contains two component beta crystal-type nucleaters, it is characterized in that polypropylene is mixed with nucleator, described nucleating agent component A is organic dibasic acid or its salt, wherein organic dibasic acid can be the phthalic acid that ortho position, contraposition or a position replace, and also can be the C of molecular formula
nH
2n(COOH)
2Aliphatic dibasic acid, n=C
1-C
10, component β is the alkaline earth metal compound of periodictable second family, the content of component A is 1 * 10 of polypropylene weight
-4-5%, the content of component B is 1 * 10 of polypropylene weight
-3-5%, melt-processed then, melt temperature is 180-300 ℃.
2, Beta-crystalline polyacrylic production method as claimed in claim 1 is characterized in that described component B is the alkaline earth metal oxide of periodictable second family, as magnesium oxide, calcium oxide, barium oxide.
3, Beta-crystalline polyacrylic production method as claimed in claim 1 is characterized in that described component B is the carbonate of the alkaline-earth metal of periodictable second family.
4, Beta-crystalline polyacrylic production method as claimed in claim 1 is characterized in that described component B is the stearate of the alkaline-earth metal of periodictable second family.
5, Beta-crystalline polyacrylic production method as claimed in claim 1 is characterized in that the beta crystal-type nucleater of described pair of component, and the content of component A is 1 * 10 of polypropylene weight
-2-1%, component B content is the 0.2-1% of polypropylene weight.
6, Beta-crystalline polyacrylic production method as claimed in claim 1 is characterized in that described melt temperature is 200-220 ℃.
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN85100465.2A CN1004076B (en) | 1985-04-01 | 1985-04-01 | Process for preparation of beta-crystalline polypropylene |
DE19863610644 DE3610644A1 (en) | 1985-04-01 | 1986-03-29 | beta -Crystalline isotactic polypropylene, process for the preparation thereof, and articles produced therefrom |
JP61071413A JPH0784502B2 (en) | 1985-04-01 | 1986-03-31 | β-Crystalline polypropylene composition or ethylene-propylene block copolymer composition and process for producing the same |
US07/308,968 US5231126A (en) | 1985-04-01 | 1989-02-09 | Beta-crystalline form of isotactic polypropylene and method for forming the same |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN85100465.2A CN1004076B (en) | 1985-04-01 | 1985-04-01 | Process for preparation of beta-crystalline polypropylene |
Publications (2)
Publication Number | Publication Date |
---|---|
CN85100465A CN85100465A (en) | 1986-07-09 |
CN1004076B true CN1004076B (en) | 1989-05-03 |
Family
ID=4791179
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN85100465.2A Expired CN1004076B (en) | 1985-04-01 | 1985-04-01 | Process for preparation of beta-crystalline polypropylene |
Country Status (3)
Country | Link |
---|---|
JP (1) | JPH0784502B2 (en) |
CN (1) | CN1004076B (en) |
DE (1) | DE3610644A1 (en) |
Cited By (1)
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WO2013097647A1 (en) | 2011-12-31 | 2013-07-04 | 广州呈和科技有限公司 | Β-crystal form nucleating agent composition for polypropylene and application thereof |
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Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS57172943A (en) * | 1981-04-17 | 1982-10-25 | Mitsui Toatsu Chem Inc | Production of beta type crystalline polypropylene |
JPS5943044A (en) * | 1982-09-06 | 1984-03-09 | Toyo Soda Mfg Co Ltd | Non-rigid propylene polymer film |
-
1985
- 1985-04-01 CN CN85100465.2A patent/CN1004076B/en not_active Expired
-
1986
- 1986-03-29 DE DE19863610644 patent/DE3610644A1/en not_active Ceased
- 1986-03-31 JP JP61071413A patent/JPH0784502B2/en not_active Expired - Lifetime
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2013097647A1 (en) | 2011-12-31 | 2013-07-04 | 广州呈和科技有限公司 | Β-crystal form nucleating agent composition for polypropylene and application thereof |
US9243123B2 (en) | 2011-12-31 | 2016-01-26 | Gch Technology Co., Ltd. | B-crystal form nucleating agent composition for polypropylene and use thereof |
Also Published As
Publication number | Publication date |
---|---|
JPS61281105A (en) | 1986-12-11 |
CN85100465A (en) | 1986-07-09 |
JPH0784502B2 (en) | 1995-09-13 |
DE3610644A1 (en) | 1986-10-02 |
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