CN1590437A - Hgdrotalcite base chlorine containing high polymer composite heat stabilizing agent - Google Patents
Hgdrotalcite base chlorine containing high polymer composite heat stabilizing agent Download PDFInfo
- Publication number
- CN1590437A CN1590437A CN 200410037656 CN200410037656A CN1590437A CN 1590437 A CN1590437 A CN 1590437A CN 200410037656 CN200410037656 CN 200410037656 CN 200410037656 A CN200410037656 A CN 200410037656A CN 1590437 A CN1590437 A CN 1590437A
- Authority
- CN
- China
- Prior art keywords
- calcium
- hydrotalcite
- zinc
- soap
- stabilizer
- 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.)
- Granted
Links
- 239000003381 stabilizer Substances 0.000 title claims description 25
- 239000002131 composite material Substances 0.000 title abstract description 16
- 229920000642 polymer Polymers 0.000 title abstract description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 title 1
- 229910052801 chlorine Inorganic materials 0.000 title 1
- 239000000460 chlorine Substances 0.000 title 1
- 229960001545 hydrotalcite Drugs 0.000 claims abstract description 44
- 229910001701 hydrotalcite Inorganic materials 0.000 claims abstract description 44
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 claims abstract description 42
- 239000000344 soap Substances 0.000 claims abstract description 19
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 9
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 9
- 239000011575 calcium Substances 0.000 claims abstract description 9
- 239000011701 zinc Substances 0.000 claims abstract description 9
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 26
- 239000011777 magnesium Substances 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 9
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 8
- 239000008116 calcium stearate Substances 0.000 claims description 8
- 235000013539 calcium stearate Nutrition 0.000 claims description 8
- 235000010237 calcium benzoate Nutrition 0.000 claims description 5
- 239000004301 calcium benzoate Substances 0.000 claims description 5
- HZQXCUSDXIKLGS-UHFFFAOYSA-L calcium;dibenzoate;trihydrate Chemical compound O.O.O.[Ca+2].[O-]C(=O)C1=CC=CC=C1.[O-]C(=O)C1=CC=CC=C1 HZQXCUSDXIKLGS-UHFFFAOYSA-L 0.000 claims description 5
- HIAAVKYLDRCDFQ-UHFFFAOYSA-L calcium;dodecanoate Chemical compound [Ca+2].CCCCCCCCCCCC([O-])=O.CCCCCCCCCCCC([O-])=O HIAAVKYLDRCDFQ-UHFFFAOYSA-L 0.000 claims description 5
- 239000011229 interlayer Substances 0.000 claims description 5
- 238000012986 modification Methods 0.000 claims description 5
- 230000004048 modification Effects 0.000 claims description 5
- 229940098697 zinc laurate Drugs 0.000 claims description 5
- JDLYKQWJXAQNNS-UHFFFAOYSA-L zinc;dibenzoate Chemical compound [Zn+2].[O-]C(=O)C1=CC=CC=C1.[O-]C(=O)C1=CC=CC=C1 JDLYKQWJXAQNNS-UHFFFAOYSA-L 0.000 claims description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 4
- 229910052749 magnesium Inorganic materials 0.000 claims description 4
- GPYYEEJOMCKTPR-UHFFFAOYSA-L zinc;dodecanoate Chemical compound [Zn+2].CCCCCCCCCCCC([O-])=O.CCCCCCCCCCCC([O-])=O GPYYEEJOMCKTPR-UHFFFAOYSA-L 0.000 claims description 4
- 150000001450 anions Chemical class 0.000 claims description 3
- HDRTWMBOUSPQON-ODZAUARKSA-L calcium;(z)-but-2-enedioate Chemical compound [Ca+2].[O-]C(=O)\C=C/C([O-])=O HDRTWMBOUSPQON-ODZAUARKSA-L 0.000 claims description 3
- ZCZLQYAECBEUBH-UHFFFAOYSA-L calcium;octadec-9-enoate Chemical compound [Ca+2].CCCCCCCCC=CCCCCCCCC([O-])=O.CCCCCCCCC=CCCCCCCCC([O-])=O ZCZLQYAECBEUBH-UHFFFAOYSA-L 0.000 claims description 3
- HJSYJHHRQVHHMQ-ODZAUARKSA-L zinc;(z)-but-2-enedioate Chemical compound [Zn+2].[O-]C(=O)\C=C/C([O-])=O HJSYJHHRQVHHMQ-ODZAUARKSA-L 0.000 claims description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 2
- 240000004528 Catalpa ovata Species 0.000 claims description 2
- 235000010005 Catalpa ovata Nutrition 0.000 claims description 2
- 239000005642 Oleic acid Substances 0.000 claims description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 2
- HRBZRZSCMANEHQ-UHFFFAOYSA-L calcium;hexadecanoate Chemical compound [Ca+2].CCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCC([O-])=O HRBZRZSCMANEHQ-UHFFFAOYSA-L 0.000 claims description 2
- NDWWLJQHOLSEHX-UHFFFAOYSA-L calcium;octanoate Chemical compound [Ca+2].CCCCCCCC([O-])=O.CCCCCCCC([O-])=O NDWWLJQHOLSEHX-UHFFFAOYSA-L 0.000 claims description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 2
- 229960002969 oleic acid Drugs 0.000 claims description 2
- 229940012185 zinc palmitate Drugs 0.000 claims description 2
- GJAPSKMAVXDBIU-UHFFFAOYSA-L zinc;hexadecanoate Chemical compound [Zn+2].CCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCC([O-])=O GJAPSKMAVXDBIU-UHFFFAOYSA-L 0.000 claims description 2
- CHJMFFKHPHCQIJ-UHFFFAOYSA-L zinc;octanoate Chemical compound [Zn+2].CCCCCCCC([O-])=O.CCCCCCCC([O-])=O CHJMFFKHPHCQIJ-UHFFFAOYSA-L 0.000 claims description 2
- 239000003017 thermal stabilizer Substances 0.000 abstract description 15
- 238000002156 mixing Methods 0.000 abstract description 10
- 239000004800 polyvinyl chloride Substances 0.000 description 36
- 229920000915 polyvinyl chloride Polymers 0.000 description 36
- 238000000034 method Methods 0.000 description 12
- 239000004709 Chlorinated polyethylene Substances 0.000 description 9
- 239000012065 filter cake Substances 0.000 description 6
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- QANIADJLTJYOFI-UHFFFAOYSA-K aluminum;magnesium;carbonate;hydroxide;hydrate Chemical compound O.[OH-].[Mg+2].[Al+3].[O-]C([O-])=O QANIADJLTJYOFI-UHFFFAOYSA-K 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- 231100000614 poison Toxicity 0.000 description 4
- 230000007096 poisonous effect Effects 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical class [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000012266 salt solution Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 235000021355 Stearic acid Nutrition 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004040 coloring Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000008117 stearic acid Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 239000004801 Chlorinated PVC Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 159000000013 aluminium salts Chemical class 0.000 description 1
- 229910000329 aluminium sulfate Inorganic materials 0.000 description 1
- 238000005844 autocatalytic reaction Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- AGXUVMPSUKZYDT-UHFFFAOYSA-L barium(2+);octadecanoate Chemical compound [Ba+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O AGXUVMPSUKZYDT-UHFFFAOYSA-L 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229920000457 chlorinated polyvinyl chloride Polymers 0.000 description 1
- KRGNPJFAKZHQPS-UHFFFAOYSA-N chloroethene;ethene Chemical group C=C.ClC=C KRGNPJFAKZHQPS-UHFFFAOYSA-N 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000000881 depressing effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229920001038 ethylene copolymer Polymers 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
- LPEBYPDZMWMCLZ-CVBJKYQLSA-L zinc;(z)-octadec-9-enoate Chemical compound [Zn+2].CCCCCCCC\C=C/CCCCCCCC([O-])=O.CCCCCCCC\C=C/CCCCCCCC([O-])=O LPEBYPDZMWMCLZ-CVBJKYQLSA-L 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
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)
Abstract
A hydrotalcite-based composite thermal stabilizer for PVC and chlorine-contained high polymer is prepared from hydrotalcite, calcium soap and zinc soap through proportionally mixing.
Description
Technical field:
The present invention relates to the chloride superpolymer composite thermal stabilizer of a kind of hydrotalcite, be specifically related to the chloride superpolymer composite thermal stabilizer of calcic/zn cpds hydrotalcite.
Background technology:
Polyvinyl chloride resin has difficult to burn, strong mechanical performance, cheap, characteristics such as raw material sources abundant, manufacturing process maturation, being widely used in industries such as building, telecommunication, traffic, electronics, chemical industry, packing, is the general thermoplastic plastic of second largest class that is only second to polyolefin.But the thermostability of PVC itself is very poor, and its yield temperature is 136 ℃, and decomposition temperature is 140 ℃, and both differ only 4 ℃, brings very big difficulty for processing and use, therefore must add the thermo-stabilizer of some amount.Other chloride superpolymer also can be heated or uviolizing under take off HCl self-catalyzed reaction, reduce the various performances of material.Thermo-stabilizer is that PVC and other chloride superpolymer are processed one of indispensable main auxiliary agent.Thermo-stabilizer mainly can be divided into base lead salt class, metallic soap class, organic tin, rare earth class and one package stabilizer etc. according to chemical structure at present.Along with environmental consciousness is strengthened, the PVC thermo-stabilizer just develops towards low toxicity, direction such as pollution-free, efficient, and research and development new generation of green environment-friendly type PVC thermo-stabilizer is significant.
Hydrotalcite claims layered double hydroxide (Layered Double Hydroxides is called for short LDHs) again, is a kind of typical anion type laminated compound, and its typical molecular composition is Mg
6Al
2(OH)
16CO
34H
2O.Because its laminate surface has alkalescence, can absorb the HCl that PVC and other chloride high polymer pyrolytics discharge, thereby play the effect that suppresses its autocatalysis Decomposition; Think in addition that in addition its thermally-stabilised mechanism is because the interchangeability of LDHs interlayer ion makes interlayer CO
3 2-Can exchange with the HCl that enters interlayer, thereby reach the effect that absorbs HCl, stablizes PVC and other chloride superpolymer.Hydrotalcite filled PVC and other thermo-stabilizers, compound as organotin, lead or zinc salt etc. as thermo-stabilizer, can further improve the thermostability of PVC.
Document [1]: United States Patent (USP) United States Patent 4299759 (1981) has reported that Japanese Kyowa chemical company took the lead in 1980 and will meet following general formula: Mg
1-xAl
x(OH)
2A
X/n N-MH
2The hydrotalcite of O (0<x≤0.5) is filled into and is used as thermo-stabilizer among the PVC, and the result has significantly improved the thermostable effect of PVC.When in 100 parts of PVC, adding 1 part of Mg
0.7Al
0.3(OH)
2(CO
3)
0.150.55H
2When O, 0.75 part of Zinic stearas and 0.3 part of organotin, the heat-stable time of PVC can be extended to 62 minutes under 180 ℃ of conditions.Equal conditions uses calcium stearate/Zinic stearas thermo-stabilizer of 2 parts down, and its heat-stable time has only 38 minutes.
Document [2]: people such as Hua Youqing [novel polyvinyl chloride thermo-stabilizer---the research of hydrotalcite, polyvinyl chloride, 2001,6:42-44] the independent hydrotalcite that uses 2 parts of Mg/Al=2 of discovery, its decomposition temperature is 264 ℃, and with hydrotalcite and organo-tin het stabilizer by after 1: 1 the mixed, in 100 parts of PVC, add 2 parts of these mixture heat stablizers, its initial decomposition temperature has been brought up to 279 ℃, has raise 15 ℃.
Document [3]: Japanese Nissan Ferro organic chemicals company's discovery perchloric acid and hydrotalcite have collaborative preferably promoter action (JP59140261,1984).They add 0.001~100 part of this composite thermal stabilizer with the hydrotalcite of 1mol and the compound back of perchloric acid of 0.001~2mol in 100 parts of polyvinyl chloride resins, can significantly improve the thermostability of PVC.For example in 100 parts of PVC, add 0.5 part of barium stearate, 0.2 part of lead salt, 0.5 part hydrotalcite/perchloric acid composite thermal stabilizer can make reach 90 minutes its steady time under 180 ℃ of conditions.
All hydrotalcite and other thermo-stabilizers have been carried out compoundly in the above-mentioned document, overcome separately hydrotalcite as the not good shortcoming of its initial coloring of thermo-stabilizer.But used poisonous elements such as lead, tin mostly, be unfavorable for that hydrotalcite replaces the development of existing price height or poisonous thermo-stabilizer fully.
Summary of the invention:
The objective of the invention is to have the shortcoming that contains poisonous elements such as lead, tin in the chloride superpolymer composite thermal stabilizer of hydrotalcite now, a kind of chloride superpolymer composite thermal stabilizer of hydrotalcite that does not contain poisonous element is provided in order to overcome.
Chloride superpolymer thermo-stabilizer provided by the invention is a kind of mixture, and its component and content are:
Hydrotalcite: 10~82%
Calcium soap: 14~95%
Zinc soap: 1~47%;
More preferably proportioning is:
Hydrotalcite: 18~57%
Calcium soap: 35~75%
Zinc soap: 4~19%
Above percentage ratio is mass percent, and these 3 kinds of component thorough mixing are obtained chloride superpolymer composite thermal stabilizer.
Calcium soap used in the present invention is a kind of in calcium stearate, calcium octoate, calcium laurate, calcium palmitate, calcium oleate, calcium benzoate, the calcium maleate, preferred calcium stearate, calcium laurate and calcium benzoate.
Zinc soap used in the present invention is a kind of in Zinic stearas, zinc octoate, zinc laurate, zinc palmitate, oleic acid Chinese catalpa, Zinc dibenzoate, the MALEIC ACID, ZINC SALT, preferred Zinic stearas, zinc laurate and Zinc dibenzoate.
Hydrotalcite used in the present invention is that interlayer anion is the magnesium aluminum-hydrotalcite of carbonate: Mg wherein
2+/ Al
3+Mol ratio satisfies 2~4: 1.Its composition should satisfy following general formula: [Mg
2+ 1-xAl
3+ x(OH)
2] CO
3 2- X/2MH
2O, wherein 0.2≤x≤0.33; 0≤m≤2.This hydrotalcite preferably passes through the organism surface modification, helps it like this and disperses in polymkeric substance.
Hydrotalcite used in the present invention can adopt the method for co-precipitation such as the pH value method that changes (claim not only single droplet method or high degree of supersaturation method), constant pH method (but also claiming two methods or low degree of supersaturation methods), nucleation/crystallization isolation method, Wyler's process, perhaps adopts methods such as hydrothermal synthesis method, roast reduction process to prepare.
Tiny in order to obtain granularity, finely dispersed hydrotalcite, the present invention has adopted nucleation/crystallization isolation method, and this method is described in detail in patent 00132145.5: concrete steps are: magnesium salts and aluminium salt are pressed Mg
2+/ Al
3+=2~4: 1 ratio is made into mixing salt solution, makes Mg
2+Concentration is 0.4~2.0mol/L; NaOH or KOH and soluble carbon hydrochlorate are pressed n (CO
3 2-)/n (Al
3+)=1.6~2.5, n (OH
-)/[n (Mg
2+)+n (Al
3+)]=1.4~2.2 ratio is made into mixing solutions, and its volume is identical with mixing salt solution.The soluble carbon hydrochlorate can be: Na
2CO
3, K
2CO
3, (NH
4)
2CO
3In any.With above-mentioned two solution short mix in the rotation liquid film reactor, the slurries that obtain after the mixing wash throw out to pH ≈ 7 at 100 ℃ of following backflow crystallization 6-10h, filter and obtain the hydrotalcite filter cake, and dry hydrotalcite filter cake obtains the hydrotalcite powder.If expect the hydrotalcite powder of surface modification, filter cake after then will washing, filtering add about 23~35 times to the water of filter cake solid content, be warming up to 80~100 ℃, add the stearic acid stirring reaction 2~5 hours of solid content 4~7%, obtain the hydrotalcite powder of surface organic after the drying.The hydrotalcite size-grade distribution that present method makes is 20nm~120nm.
Composite thermal stabilizer provided by the present invention is mainly used in the chloride superpolymer, polyvinyl chloride normally, chlorinatedpolyethylene, chlorinated polyvinyl chloride, vinyl chloride-ethylene copolymer, vinyl chloride acetate copolymer etc.Thermo-stabilizer addition (according to the mass fraction) is advisable to add 0.1~10 part in 100 parts of chloride superpolymer, and preferable addition is 3~6 parts.
By polyvinyl chloride and the chlorinatedpolyethylene (CPE) that adds above-mentioned composite thermal stabilizer carried out the static heat senile experiment, the result shows that composite thermal stabilizer provided by the present invention can effectively improve the thermostability of PVC and other chloride superpolymer.Under 180 ± 1 ℃ of environment, PVC and chloride superpolymer have shown initial coloring preferably, and heat-stable time can reach more than 80~220 minutes, and PVC and its heat-stable time of chloride superpolymer of not adding thermo-stabilizer have only 6~10 minutes.
Embodiment:
Embodiment 1~9
Take by weighing 48.15g MgSO respectively
4(0.4mol) and 66.64gAl
2(SO
4)
318H
2O (0.1mol) mixes the back and adds deionized water and prepare Mg to 500ml
2+/ Al
3+Mole is 2 mixed salt solution; Take by weighing 42.4gNa
2CO
3(0.4mol) and 38.4gNaOH (0.96mol) add deionized water and prepare mixed ammonium/alkali solutions to 500ml, CO in the alkaline solution
3 2-And OH
-Volumetric molar concentration satisfy n (CO respectively
3 2-)/n (Al
3+)=2, n (OH
-)/[n (Mg
2+)+n (Al
3+)]=1.6.With above-mentioned two kinds of solution short mix in the rotation liquid film reactor, the slurries that obtain after the mixing are at 100 ℃ of following backflow crystallization 6h, throw out washs to pH ≈ 7 and obtains the hydrotalcite filter cake, add about 30 times to the water of filter cake solid content, be warming up to 80 ℃, the stearic acid stirring reaction of adding solid content 5% 2 hours, the magnesium/aluminum ratio that can obtain surface modification after the drying is 2 hydrotalcite powder.
As stated above, change MgSO
4And Al
2(SO
4)
318H
2The amount of O makes Mg in the mixing solutions
2+/ Al
3+Mol ratio is respectively 2.5,3,3.5,4 and can obtains magnesium/aluminum ratio and be respectively 2.5,3,3.5,4 surface modification hydrotalcite powder.
With respectively with above-mentioned hydrotalcite and calcium stearate, Zinic stearas by 30%, 60%, 10% mixed, obtain chloride superpolymer composite thermal stabilizer.The composite thermal stabilizer of different amounts is added among 100 parts of PVC or the CPE, add 50 parts of dimixo-octyl phthalates (DOP) again, on SSR-Z4 plastic experimental machine in 140 ℃ mixing 10 minutes, depressing to thickness 100 ℃ of conditions is the thin slice of 1mm and the test piece that is cut into 1cm * 1cm.Place 180 ± 1 ℃ heat aging test chamber to carry out static-aging experiment test piece, test piece is begun and time that the black point solution point occurs is decided to be heat-stable time, the result is as shown in table 1:
Table 1
Embodiment | ??Mg/Al | Superpolymer (100 parts) | Thermo-stabilizer (part) | Heat-stable time (minute) |
????1 | ????2 | ????PVC | ????0 | ????7 |
????2 | ????2 | ????CPE | ????0 | ????9 |
????3 | ????2 | ????PVC | ????1 | ????160 |
????4 | ????2 | ????PVC | ????2 | ????200 |
????5 | ????2.5 | ????PVC | ????2 | ????190 |
????6 | ????3 | ????PVC | ????2 | ????170 |
????7 | ????3 | ????CPE | ????5 | ????190 |
????8 | ????3.5 | ????PVC | ????8 | ????180 |
????9 | ????4 | ????CPE | ????2 | ????90 |
Embodiment 10~15
Change the composition and the ratio of composite thermal stabilizer, add in 100 parts of PVC or other the chloride superpolymer by different amounts, carry out mixing, compressing tablet after adding 50 parts of DOP, carry out static-aging and test in 180 ± 1 ℃ heat aging test chamber, the result is as shown in table 2:
Table 2
Embodiment | ??Mg/Al | Superpolymer (100 parts) | Thermo-stabilizer is formed and proportioning | Thermo-stabilizer consumption (part) | Heat-stable time (minute) |
????10 | ????2 | ??PVC | 33%+51%+16% (hydrotalcite+calcium stearate+Zinic stearas) | ????3 | ????190 |
????11 | ????2 | ??PVC | 46%+46%+8% (hydrotalcite+calcium laurate+zinc laurate) | ????4 | ????170 |
????12 | ????2 | ??PVC | 11%+85%+4% (hydrotalcite+calcium oleate+zinc oleate) | ????5 | ????120 |
????13 | ????2 | ??CPE | 10%+80%+10% (hydrotalcite+calcium maleate+MALEIC ACID, ZINC SALT) | ????2 | ????90 |
????14 | ????3 | ??PVC | 69%+28%+3% (hydrotalcite+calcium stearate+Zinic stearas) | ????7 | ????210 |
????15 | ????3 | ??CPE | 44%+44%+12% (hydrotalcite+calcium benzoate+Zinc dibenzoate) | ????9 | ????200 |
Claims (4)
1. chloride superpolymer thermo-stabilizer, by the mixture that hydrotalcite, calcium soap and zinc soap are formed, the proportioning of each component is:
Hydrotalcite: 10~82%
Calcium soap: 14~95%
Zinc soap: 1~47%
Above percentage ratio is mass percent;
Wherein calcium soap is a kind of in calcium stearate, calcium octoate, calcium laurate, calcium palmitate, calcium oleate, calcium benzoate, the calcium maleate;
Zinc soap is a kind of in Zinic stearas, zinc octoate, zinc laurate, zinc palmitate, oleic acid Chinese catalpa, Zinc dibenzoate, the MALEIC ACID, ZINC SALT;
Hydrotalcite is that interlayer anion is the magnesium aluminum-hydrotalcite of carbonate: its Mg
2+/ Al
3+Mol ratio should satisfy 2~4: 1, and its composition should satisfy following general formula: [Mg
2+ 1-xAl
3+ x(OH)
2] CO
3 2- X/2MH
2O, wherein 0.2≤x≤0.33; 0≤m≤2.
2. chloride superpolymer thermo-stabilizer as claimed in claim 1 is characterized in that the ratio of each component is:
Hydrotalcite: 18~57%
Calcium soap: 35~75%
Zinc soap: 4~19%
Above percentage ratio is mass percent;
Calcium soap is calcium stearate, calcium laurate and calcium benzoate; Zinc soap is Zinic stearas, zinc laurate and Zinc dibenzoate; Hydrotalcite is 20nm~120nm hydrotalcite through organism surface modification, granularity.
3. chloride superpolymer thermo-stabilizer as claimed in claim 1 is characterized in that its addition in chloride superpolymer is to add 0.1~10 mass parts in the chloride superpolymer of per 100 mass parts.
4. chloride superpolymer thermo-stabilizer as claimed in claim 1 is characterized in that its addition in chloride superpolymer is to add 3~6 mass parts in the chloride superpolymer of per 100 mass parts.
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CN 200410037656 CN1252159C (en) | 2004-04-29 | 2004-04-29 | Hgdrotalcite base chlorine containing high polymer composite heat stabilizing agent |
PCT/CN2004/001113 WO2005105909A1 (en) | 2004-04-29 | 2004-09-28 | A hydrotalcite-based composite heat stabilizer for chlorine-containing high polymer |
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CN 200410037656 CN1252159C (en) | 2004-04-29 | 2004-04-29 | Hgdrotalcite base chlorine containing high polymer composite heat stabilizing agent |
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