CN102746595B - Method for preparing modified liquid metal soap thermal stabilizer through potassium ion characteristic doping - Google Patents
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- 239000000344 soap Substances 0.000 title claims abstract description 33
- 229910001338 liquidmetal Inorganic materials 0.000 title claims abstract description 32
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 229910001414 potassium ion Inorganic materials 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000003017 thermal stabilizer Substances 0.000 title abstract description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 30
- 239000007788 liquid Substances 0.000 claims abstract description 29
- 239000002131 composite material Substances 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 150000007524 organic acids Chemical class 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 8
- 238000004821 distillation Methods 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 5
- 239000003381 stabilizer Substances 0.000 claims description 33
- 239000012760 heat stabilizer Substances 0.000 claims description 14
- 238000002360 preparation method Methods 0.000 claims description 12
- KDVYCTOWXSLNNI-UHFFFAOYSA-N 4-t-Butylbenzoic acid Chemical compound CC(C)(C)C1=CC=C(C(O)=O)C=C1 KDVYCTOWXSLNNI-UHFFFAOYSA-N 0.000 claims description 8
- OEOIWYCWCDBOPA-UHFFFAOYSA-N 6-methyl-heptanoic acid Chemical compound CC(C)CCCCC(O)=O OEOIWYCWCDBOPA-UHFFFAOYSA-N 0.000 claims description 8
- 230000007613 environmental effect Effects 0.000 claims description 8
- 229910021645 metal ion Inorganic materials 0.000 claims description 6
- 230000004044 response Effects 0.000 claims description 6
- 239000003350 kerosene Substances 0.000 claims description 5
- 230000009967 tasteless effect Effects 0.000 claims description 5
- 239000012530 fluid Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 239000003112 inhibitor Substances 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 238000003786 synthesis reaction Methods 0.000 claims description 3
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000004593 Epoxy Substances 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 125000001931 aliphatic group Chemical group 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 150000004702 methyl esters Chemical class 0.000 claims description 2
- -1 phosphorous acid ester Chemical class 0.000 claims description 2
- 230000006641 stabilisation Effects 0.000 claims description 2
- 238000011105 stabilization Methods 0.000 claims description 2
- 230000002195 synergetic effect Effects 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 230000033228 biological regulation Effects 0.000 claims 1
- 239000004800 polyvinyl chloride Substances 0.000 abstract description 27
- 229920000915 polyvinyl chloride Polymers 0.000 abstract description 26
- 239000011701 zinc Substances 0.000 abstract description 12
- 230000008569 process Effects 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 238000011160 research Methods 0.000 abstract description 4
- 150000003839 salts Chemical class 0.000 abstract description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 230000007774 longterm Effects 0.000 abstract description 2
- 238000003889 chemical engineering Methods 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 239000012847 fine chemical Substances 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 230000005764 inhibitory process Effects 0.000 abstract 1
- 231100000956 nontoxicity Toxicity 0.000 abstract 1
- 238000005580 one pot reaction Methods 0.000 abstract 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 abstract 1
- 238000011085 pressure filtration Methods 0.000 abstract 1
- 238000001308 synthesis method Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 7
- 238000004500 asepsis Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 4
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 4
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 4
- 239000005642 Oleic acid Substances 0.000 description 4
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000006260 foam Substances 0.000 description 4
- 229910001385 heavy metal Inorganic materials 0.000 description 4
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 4
- 239000002932 luster Substances 0.000 description 4
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 238000012827 research and development Methods 0.000 description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- XVYHFPMIBWTTLH-UHFFFAOYSA-N [Zn].[Mg].[Ca] Chemical compound [Zn].[Mg].[Ca] XVYHFPMIBWTTLH-UHFFFAOYSA-N 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000002608 ionic liquid Substances 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- MNAHQWDCXOHBHK-UHFFFAOYSA-N 1-phenylpropane-1,1-diol Chemical compound CCC(O)(O)C1=CC=CC=C1 MNAHQWDCXOHBHK-UHFFFAOYSA-N 0.000 description 1
- 239000004135 Bone phosphate Substances 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 1
- NFVZIERLAZUYBQ-UHFFFAOYSA-N [K].[Zn] Chemical compound [K].[Zn] NFVZIERLAZUYBQ-UHFFFAOYSA-N 0.000 description 1
- 150000007933 aliphatic carboxylic acids Chemical class 0.000 description 1
- 239000005030 aluminium foil Substances 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 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
- MGFRKBRDZIMZGO-UHFFFAOYSA-N barium cadmium Chemical compound [Cd].[Ba] MGFRKBRDZIMZGO-UHFFFAOYSA-N 0.000 description 1
- SHLNMHIRQGRGOL-UHFFFAOYSA-N barium zinc Chemical compound [Zn].[Ba] SHLNMHIRQGRGOL-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 231100000734 genotoxic potential Toxicity 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000008447 perception Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 239000000843 powder Substances 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
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to a method for preparing a modified liquid metal soap thermal stabilizer through potassium ion characteristic doping, belonging to the technical fields of fine chemical engineering and high molecular material application. The invention researches and develops a potassium-ion-doped PVC (polyvinyl chloride) liquid metal soap thermal stabilizer. The synthesis method of the thermal stabilizer comprises the following steps: adding composite organic acid into a three-neck flask, stirring, and heating to 90-100 DEG C; adding solid potassium hydroxide in batches; after the reaction is complete, performing reduced-pressure distillation to dewater; cooling to 80 DEG C, then adding a liquid metal soap and a solvent, and continuously stirring to react; and finally, performing reduced-pressure filtration to obtain a yellowish transparent oily liquid. By utilizing the fact that metal potassium salt has fine long-term thermal stability, produces an obviously strong inhibition effect on zinc burning and has obvious cooperativity with other metal salt, the potassium-ion-doped PVC liquid metal soap thermal stabilizer is directly prepared through a solid-liquid one-step reaction method. The thermal stabilizer has the advantages of low cost, no toxicity, environment friendliness, simple process, fine performance, light appearance color and the like, and is easy to popularize and apply.
Description
Technical field
A kind of preparation method who utilizes the property doped modified liquid metal soap of potassium ion of the present invention, is specifically related to a kind of PVC liquid heat stabilizer and preparation method of doped with potassium ion, belongs to fine chemistry industry and macromolecular material applied technical field.
Background technology
Polyvinyl chloride (PVC) is China first, second-biggest-in-the-world synthetic resins, have the advantages such as cheap, difficulty is fired, corrosion-resistant and properties of transparency good, electrical insulating property is good, but the disadvantage of PVC is poor heat stability.In PVC processing, must add certain thermo-stabilizer to improve performance.Industrialized PVC thermo-stabilizer mainly contains lead salts in the world at present, hybrid metal salt, organic tin, antimony organic class, organic auxiliary heat stabilizer, rare earth class.The be still traditional lead system, barium system, cadmium of world PVC thermo-stabilizer output maximum are class stablizer.But the impact that this type of toxic heavy metal thermo-stabilizer is improved constantly by RoHS instruction and EUP instruction technique barrier and Chinese environmental protection requirement, share of market will constantly decline, and have the trend being eliminated.
In recent years due to the increase gradually of PVC material usage, the kind of thermo-stabilizer is also constantly pushing away newly, be accompanied by China's economy, social sustainable development, people's environmental consciousness and health perception strengthen day by day, and nontoxic, pollution-free, compound and efficient composite thermal stabilizer has become the developing direction of PVC thermo-stabilizer in world wide.The new liquid thermo-stabilizer of the advantages such as particularly have no dust pollution, metering is simple, and environmental protection low price and technique are simple has become the developing direction of following macromolecular material thermo-stabilizer.
The liquid metal salt heat stabilizers of asepsis environment-protecting is in China also in development, and research is at present still immature, and it is high that the product on market has cost, environmental protection not, and stability is bad, the shortcomings such as appearance luster is dark, complex process.Application number is that 201010517144.6 patent is reacted aliphatic carboxylic acid, aromatic carboxylic acid and oleic acid with the oxyhydroxide of calcium magnesium zinc, finally logical N
2discharge oleic acid, obtain liquid tribasic calcium magnesium zinc heat stabilizer, the method is led to N
2discharge oleic acid, need high temperature to discharge oleic acid, complex process, suitability for industrialized production is difficulty comparatively.Application number be 201010104069.0 patent system standby have the liquid barium zinc heat stabilizer of heavy metal, and added dihydroxyphenyl propane and made oxidation inhibitor, double A is a kind of clearly toxic substance of forbidding, has seriously limited the application of this liquid stabilisers in field of Environment Protection.
The research of potassium zinc liquid heat stabilizer is also in the initial stage at present, the present invention utilizes the good characteristic of potassium ion, by doped with potassium ion, prepare liquid polyhydric metal soap, it has been simplified synthesis technique, has reduced production cost, asepsis environment-protecting, substitute liquid heat stabilizer Ba/Zn, the Ba/Cd/Zn etc. of tradition containing toxic heavy metal, improved the various defects of traditional thermo-stabilizer production process, the research and development frontier of having opened up asepsis environment-protecting liquid heat stabilizer; The novel doped with potassium ionic liquid metal soap of preparation not only has good thermal stability, also with certain foam performance, particularly good thermal stability and the foam performance of Liquid K zinc metallic soap, having accomplished the multiplex effect of potion in formula, is the multiplex new focus of current auxiliary agent research potion; Its appearance luster of doped with potassium ionic liquid metal soap of preparation is shallow, can be used in various transparent articles and white goods, and Application Areas is extensive, has wide market outlook.
Summary of the invention
The object of the invention is to provide a kind of PVC liquid metal soap thermo-stabilizer and preparation method of doped with potassium ion, this thermo-stabilizer has high-efficiency environment friendly, simple to operate, produce low cost, process safety and good thermal stability and foam performance, the complex manufacturing, stability and the consistency that have overcome traditional field thermo-stabilizer are poor, color and luster is dark, cost is high and shortcoming and the production technology defect such as genotoxic potential, have opened up the frontier of asepsis environment-protecting liquid heat stabilizer research and development.
Technical scheme of the present invention: a kind of preparation method of PVC liquid metal soap thermo-stabilizer of doped with potassium ion, its synthesis step is as follows:
(1) in 250mL there-necked flask, add successively composite organic acid, constantly stir and be warming up to 90-100 ℃;
Described composite organic acid is isocaprylic acid and p-tert-butyl benzoic acid, and the mass percent containing isocaprylic acid in composite organic acid is 40% ~ 70%, and the mass percent that contains p-tert-butyl benzoic acid is 30% ~ 60%;
(2) reaction temperature control 90-100 ℃, adds solid potassium hydroxide in batches, and potassium hydroxide add-on is the 15%-40% of composite organic acid quality, after question response is thorough, carries out underpressure distillation and dewaters;
(3) add liquid metal soap and solvent after being cooled to 80 ℃, carry out decompress filter after stirring 10min, to forming uniform and stable transparent oily liquid, be the PVC liquid metal soap thermo-stabilizer of product doped with potassium ion;
Described liquid metal soap is one or more mixtures in independent Zn, Ca/Zn, Mg/Zn and Al/Zn;
Add liquid metal soap quality be 45% ~ 80% of composite organic acid quality;
Described solvent is any one or multiple mixture in triglycol, tasteless kerosene, 25# transformer oil, whiteruss; The quality of institute's solubilizing agent is 60% ~ 95% of composite organic acid quality.
In building-up process, by regulating and controlling the quality that adds of liquid metal soap and solvent, regulate and control metal ion mass ratio, draw the metal ion ratio of cooperation thermal stabilization best performance.
Utilize the preparation method of the PVC liquid metal soap thermo-stabilizer of doped with potassium ion, this reaction adopts composite organic acid and the direct solid-liquid single step reaction of solid potassium hydroxide method, overcomes the technological deficiency of traditional processing technology complexity.
Utilizing the preparation method of the PVC liquid metal soap thermo-stabilizer of doped with potassium ion, in building-up process, can be that micro-yellow is to linen liquid heat stabilizer according to regulating metal ion mass ratio, making outward appearance.
A kind of preparation method of environmental protection composite fluid thermo-stabilizer of the PVC liquid metal soap thermo-stabilizer that contains described doped with potassium ion, the PVC liquid metal soap thermo-stabilizer of the doped with potassium ion of preparing by described method, add again liquid type auxiliary heat stabilizer: one or more in oxidation inhibitor, epoxy aliphatic acid methyl ester, phosphorous acid ester, liquid beta-diketon etc. are carried out polynary composite, make the novel environment friendly composite fluid thermo-stabilizer that consistency and synergistic effect are good.
Beneficial effect of the present invention: (1) has prepared a kind of PVC liquid metal soap thermo-stabilizer of novel doped with potassium ion, wherein potassium ion has good long-term thermal stability energy, there is obvious synergisticing performance with other metal ions, show higher thermal stability and certain foam performance.(2) high, the high-efficiency environment friendly of this thermo-stabilizer quality product, containing poisonous heavy metal, appearance luster is shallow, be widely used; Process safety, simple to operate, be suitable for industrialized production; Raw material is easy to get, and energy consumption is little, and cost is low, and three-waste free pollution meets requirement and the energy-saving and emission-reduction demand of current Chemicals environmental protection completely.(3) overcome performance shortcomings and the production technology defect of traditional thermo-stabilizer, opened up the frontier of asepsis environment-protecting liquid heat stabilizer research and development, there are wide market outlook.
Embodiment
The following examples are to further elaboration of the present invention, but the invention is not restricted to this.
Embodiment 1
In 250mL there-necked flask, add successively 43.2g isocaprylic acid, 26.8g p-tert-butyl benzoic acid, under constantly stirring, be heated to 90 ℃, 90 ℃ of reaction temperature controls, add 14.0g solid potassium hydroxide in batches, thorough to reaction, solution becomes clarification, carries out underpressure distillation and dewaters; Add in batches 32.6g Zinc oxide powder, 80 ℃ of reaction 1h of temperature control, after question response is complete, add tasteless kerosene 54g, continue to carry out decompress filter after temperature control stirring 10min, obtain yellowish transparent oily liquid, and sealing is preserved.
Embodiment 2
In 250mL there-necked flask, add successively 28.8g isocaprylic acid, 17.0g p-tert-butyl benzoic acid, under constantly stirring, be heated to 100 ℃, 100 ℃ of reaction temperature controls, add 16.6g potassium hydroxide in batches, temperature control reaction 2h, after question response is complete, carries out underpressure distillation dehydration; Until anhydrous, stop distilling and be cooled to 80 ℃ after deviating from, adding 28.5g liquid Ca/Zn composite thermal stabilizer and triglycol 30g, continuing to carry out decompress filter after temperature control stirring 10min, obtaining yellowish transparent oily liquid, sealing is preserved.
Embodiment 3
In 250mL there-necked flask, add successively 14.2g isocaprylic acid, 17.5g p-tert-butyl benzoic acid, under constantly stirring, be heated to 90 ℃, 90 ℃ of reaction temperature controls, add 11.0g potassium hydroxide in batches, temperature control reaction 2h, after question response is complete, carries out underpressure distillation dehydration; Until anhydrous, stop distilling and be cooled to 80 ℃ after deviating from, adding 25.0g liquid Mg/Zn composite thermal stabilizer and tasteless kerosene 24g, continuing to carry out decompress filter after temperature control stirring 10min, obtaining flavous transparent oily liquid, sealing is preserved.
Embodiment 4
In 250m there-necked flask, add successively 14.6g isocaprylic acid, 8.8g p-tert-butyl benzoic acid, under constantly stirring, be heated to 90 ℃, 90 ℃ of reaction temperature controls add 7.9g potassium hydroxide in batches, and temperature control reaction 1h, after question response is complete, carries out underpressure distillation and dewater; Until anhydrous, stop distilling and be cooled to 80 ℃ after deviating from, adding 17.4g liquid A l/Zn composite thermal stabilizer and tasteless kerosene 16g, continuing to carry out decompress filter after temperature control stirring 10min, obtaining linen transparent oily liquid, sealing is preserved.
50 parts, PVC powder, PVC are stuck with paste to 50 parts of resins, 50 parts of DOP, 3 parts of thermo-stabilizers, in 120 ℃ of baking ovens, plastify 20 min, after taking-up, make thickness and be about the test piece of 1mm, according to GB/T9349-2002, test piece is cut into the square of 15mm * 15mm, be positioned on clean aluminium foil, in the air dry oven of 180 ℃, heat, every 5min or 10min get a PVC test piece, thereby observe the variation of test piece color, result is as shown in table 1.
Table 1 oven heat method test result
The blank PVC of 1-, 2-adds the PVC of the PVC liquid metal soap thermo-stabilizer of self-control doped with potassium ion, and 3-adds the PVC of barium cadmium Zn composite heat stabilizer on market
The quality index of the PVC liquid metal soap thermo-stabilizer product of table 2 doped with potassium ion
Claims (2)
1. a preparation method for the PVC liquid metal soap thermo-stabilizer of doped with potassium ion, is characterized in that synthesis step is:
(1) in 250mL there-necked flask, add successively composite organic acid, constantly stir and be warming up to 90-100 ℃;
Described composite organic acid is isocaprylic acid and p-tert-butyl benzoic acid, and the mass percent containing isocaprylic acid in composite organic acid is 40% ~ 70%, and the mass percent that contains p-tert-butyl benzoic acid is 30% ~ 60%;
(2) reaction temperature control 90-100 ℃, adds solid potassium hydroxide in batches, and potassium hydroxide add-on is the 15%-40% of composite organic acid quality, after question response is complete, carries out underpressure distillation and dewaters;
(3) add liquid metal soap and solvent after being cooled to 80 ℃, carry out decompress filter after stirring 10min, to forming uniform and stable transparent oily liquid, be the PVC liquid metal soap thermo-stabilizer of product doped with potassium ion;
Described liquid metal soap is one or more mixtures in independent Zn, Ca/Zn, Mg/Zn and Al/Zn; And add liquid metal soap quality be 45% ~ 80% of composite organic acid quality;
Described solvent is any one or multiple mixture in triglycol, tasteless kerosene, 25# transformer oil, whiteruss; And the quality of institute's solubilizing agent is 60% ~ 95% of composite organic acid quality;
The quality that adds by regulation and control liquid metal soap and solvent regulates and controls metal ion mass ratio, draws the metal ion ratio of cooperation thermal stabilization best performance.
2. the preparation method of the environmental protection composite fluid thermo-stabilizer of a PVC liquid metal soap thermo-stabilizer that contains doped with potassium ion claimed in claim 1, it is characterized in that: the PVC liquid metal soap thermo-stabilizer of the doped with potassium ion of preparing by method described in claim 1, add again liquid type auxiliary heat stabilizer: one or more in oxidation inhibitor, epoxy aliphatic acid methyl ester, phosphorous acid ester, liquid beta-diketon are carried out polynary composite, make the environmental protection composite fluid thermo-stabilizer that consistency and synergistic effect are good.
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| CN105921688A (en) * | 2016-06-07 | 2016-09-07 | 平顶山市美伊金属制品有限公司 | Composite release agent for die casting of metal cooker and preparation method thereof |
| CN105921687A (en) * | 2016-06-07 | 2016-09-07 | 平顶山市美伊金属制品有限公司 | Casting release agent for producing cast iron pan and preparation method thereof |
| CN109467931B (en) * | 2017-09-07 | 2020-10-02 | 北京化工大学 | Flexible dielectric elastomer composite material based on nano liquid metal and preparation method thereof |
| CN109439290B (en) * | 2018-12-05 | 2021-03-16 | 山东恒利热载体工程技术有限公司 | Environment-friendly organic heat carrier and preparation method thereof |
| CN111205514A (en) * | 2020-03-12 | 2020-05-29 | 德清县东来化学有限公司 | Sodium potassium zinc liquid stabilizer and preparation method and application thereof |
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|---|---|---|---|---|
| BR8907113A (en) * | 1988-10-07 | 1991-02-05 | M & T Chemicals Inc | STABILIZING COMPOSITION, THERMOPLASTIC POLYMER COMPOSITION, ARTICLE AND PROCESS TO STABILIZE A THERMOPLASTIC COMPOSITION |
| JPH05262942A (en) * | 1992-03-19 | 1993-10-12 | Asahi Denka Kogyo Kk | Chlorine-containing resin composition |
| CN102086271B (en) * | 2010-12-15 | 2012-10-10 | 浙江传化华洋化工有限公司 | Preparation method of high-transparent high heat resistance liquid calcium-zinc heat stabilizer |
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2012
- 2012-07-19 CN CN201210250155.1A patent/CN102746595B/en not_active Expired - Fee Related
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