CN106432957A - Preparation and application of zinc cyanurate/zinc uracil compound efficient PVC stabilizer - Google Patents
Preparation and application of zinc cyanurate/zinc uracil compound efficient PVC stabilizer Download PDFInfo
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- CN106432957A CN106432957A CN201610850208.1A CN201610850208A CN106432957A CN 106432957 A CN106432957 A CN 106432957A CN 201610850208 A CN201610850208 A CN 201610850208A CN 106432957 A CN106432957 A CN 106432957A
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention relates to a zinc cyanurate/zinc uracil compound efficient PVC stabilizer used for improving the PVC heat stability. The zinc cyanurate/zinc uracil compound efficient PVC stabilizer is prepared from, by weight, 80-90 parts of zinc cyanurate, 10-20 parts of zinc uracil, 2-5 parts of plasticizer, 1-2 parts of dispersant and 2-5 parts of antioxygen. A certain amount of zinc cyanurate, a certain amount of zinc uracil and a certain amount of antioxygen are mixed in a high-speed mixer at high speed, a proper amount of dispersant and a proper amount of plasticizer are sequentially added in the mixing process, high-speed mixing is carried out for 5-10 min, and powder in a cavity is evenly mixed. According to the zinc cyanurate/zinc uracil compound efficient PVC stabilizer, the stability of the PVC material in the processing process is remarkably improved, compared with a traditional lead salt stabilizer and a traditional calcium-zinc stabilizer, high heat stability is achieved, the initial colorability of PVC is reduced, later zinc burning is prolonged, the raw materials are easy to obtain, and the preparation process is simple. Thus, good industrial application prospects are achieved, and the zinc cyanurate/zinc uracil compound efficient PVC stabilizer is suitable for industrial mass production.
Description
Technical field
The present invention relates to a kind of preparation and application of cyanuric acid zinc/efficient PVC stabilizer of urea pyrimidine zinc Compositional type, the present invention
It is related to cyanuric acid zinc/new application in terms of PVC thermal stability for the efficient PVC stabilizer of urea pyrimidine zinc Compositional type.
Background technology
Commonly use PVC heat stabilizer at present with the heat stabilizer containing metal ion such as lead salts, metal soap, organic tin
Based on.With the enhancing of mankind's environmental consciousness, just starting research and development Environment-friendlyheat heat stabilizer both at home and abroad to replace traditional non-environmental protection
The upsurge of kind.Pure organic heat stabilizers do not contain metallic element, are current novel environment friendly heat stabilizer research and development focus.
As other chemicals, the production application of traditional heat stabilizer also can endanger human health and human survival
Environment.So, people start to start exploitation popularization non-toxic heat stabilizer to replace the upsurge of traditional poisonous kind.Among these with
The heat stabilizer that organic compound is entirely free of the organic compound base of any metal as main stabilizer represents PVC heat surely
Determine the long term growth direction of agent industry, develop the forefront field that pure organic main stabilizer is thermally-stabilised research and development at present.
Chinese patent CN105315574 A have studied a kind of PVC calcium zinc heat stabilizer and its application, by quinolone zinc salt
Compound composition with quinolone calcium salt, although this PVC calcium zinc heat stabilizer has good thermal stability, and preferably
Antibacterial surface function, but this technique productions high cost, unsuitable industrialized production.In existing numerous organic heat stabilizers,
Most of only have absorption HCl, be complexed the functions such as the metal chloride with catalysis PVC degraded.However, PVC heat stabilizer
In the middle of function, the ability replacing unstable chlorine atom is only most critical.Absorb the degraded that the abilities such as HCl can only delay PVC, and
Replacement unstable chlorine atomic energy eliminates at the very start and causes PVC degradation factors to stop PVC from degrading.Although what oneself developed at present contains
The ability that nitrogen type thermal stabilizing agent replaces unstable chlorine atom is weaker, also cannot use as main stabilizer, but it has remained
The most potential kind developing into main stabilizer in machine heat stabilizer.
Lead salt stabilizer is that in the middle of all stabilizers, cost performance highest is a kind of, and always in occupation of leading position,
Due to its excellent transparency, good initial coloring is also frequently used European good fortune soaps stabilizer.In whole world green
Under the pressure of peace movement, because lead, good fortune class stabilizer are poisonous and its significant damage that environment is caused, countries in the world go out one after another
The platform new measure, limits or forbids the use of lead, cadmium stabilizer in PVC production process, and the process to PVC discarded object is formulated
Strict regulations.
There are some researches show, Chinese patent CN101901076A with fatty alcohol or organic acid, acylate, epoxidized soybean oil,
Micro-nano metal and sepiolite or inorganic non-metallic breeze, the stabilizer of composition, this stabilizer removes has conventional stabilizer
Stabilization outside, also to resin converted products, there is toughness reinforcing enhancing, fire-retardant and high-weatherability, but post processing be complicated,
Energy consumption is excessive, is unfavorable for cost-effective.Calcium zinc heat stabilizer is typical case's generation of nonhazardous auxiliary agent in polyvinyl chloride (PVC) industry
Table.And, compared with organo-tin het stabilizer, calcium zinc is generally tasteless, the relatively low advantage of cost.Thus, become PVC Auxiliaries Industry
Important research field.One of research contents of calcium zinc heat stabilizer is to improve it to thermal stability of both PVC simultaneously:Just
Phase tinctorial property and drastically aging (" the zinc burning ") in later stage.
The present invention describes a kind of zinc-containing raw materials use being formed with cyanuric acid zinc/efficient PVC stabilizer of urea pyrimidine zinc Compositional type
To improve PVC thermal stability, this application scheme has no that relevant document discloses.
Content of the invention
The present invention relates to stablizing for improving the efficient PVC that the cyanuric acid zinc/urea pyrimidine zinc of PVC thermal stability compounds
Agent, raw material weight proportioning of soup processed is:80 ~ 90 parts of cyanuric acid zinc, 10 ~ 20 parts of urea pyrimidine zinc, 2 ~ 5 parts of plasticizer, 1 ~ 2 part of dispersant, resist
2 ~ 5 parts of oxygen agent.A certain amount of cyanuric acid zinc, urea pyrimidine zinc and antioxidant are placed in the mixing of high mixer high speed, in mixed process
In sequentially add appropriate dispersant and plasticizer, mixed at high speed 5 ~ 10min, so that the powder of within the chamber is uniformly mixed, then will
PVC is placed in 160 DEG C of roller temperature with the material after a certain amount of mixing, and the double roller plastic-making device of roll spacing is plasticated 5min, after taking piece, is cut into
2cm × 2cm blockage sample, according to ASTM D1925-70 standard, records its yellowness index.
A kind of preparation and application of described cyanuric acid zinc/efficient PVC stabilizer of urea pyrimidine zinc Compositional type, its feature exists
In:Described plasticizer is dioctyl phthalate, di-n-octyl phthalate, BBP(Butyl Benzyl Phthalate, O-phthalic
One or more of sour di-sec-octyl, dicyclohexyl phthalate.
A kind of preparation and application of described cyanuric acid zinc/efficient PVC stabilizer of urea pyrimidine zinc Compositional type, its feature exists
In:Described dispersant is one or more of epoxidized soybean oil, castor oil, silicone oil.
A kind of preparation and application of described cyanuric acid zinc/efficient PVC stabilizer of urea pyrimidine zinc Compositional type, its feature exists
In:Described antioxidant includes β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid positive octadecanol ester, phenyl salicylate, phosphorous
Sour three (2,4- di-tert-butyl-phenyl) ester, one or more of 1010,1076.
A kind of preparation and application of cyanuric acid zinc/efficient PVC stabilizer of urea pyrimidine zinc Compositional type it is characterised in that according under
Row step is carried out:A certain amount of cyanuric acid zinc, urea pyrimidine zinc and antioxidant are placed in the mixing of high mixer high speed, in mixed process
In sequentially add appropriate dispersant and plasticizer, mixed at high speed 10min, so that the powder of within the chamber is uniformly mixed.
Beneficial effect:
Uracil zinc polycarboxylate is a kind of organo-alkali compound containing zinc, and carbon-alkoxylation displacement pi-allyl both can occur
Chlorine atom, unstable chlorine atom is eliminated from PVC macromolecular main chain;Absorption PVC can also be neutralized discharge because of thermal degradation
HCl, play suppression PVC thermal decomposition effect.This uracil zinc polycarboxylate chemical combination that the present invention provides can change effectively simultaneously
The initial coloring of kind PVC and long-term thermal stability performance.
The PVC sample employing cyanuric acid zinc has preferable thermal stability, and stabilization time is close to four times of pure PVC sample
And the twice containing Ca/Zn sample.It is known that lead salt stabilizer is the extraordinary stabilizer of first stability effect, simply
Because poisonous usage amount in recent years just slowly reduces.And the efficient PVC that the cyanuric acid zinc prepared by this patent/urea pyrimidine zinc compounds
The stablizing effect of stabilizer is suitable with the stabilizer effect of lead salts, illustrates that the efficient PVC that cyanuric acid zinc/urea pyrimidine zinc compounds is steady
Determine the ability that agent has very strong absorption HCl, can significantly improve the thermal stability of PVC, so that PVC is reduced initial coloration and prolong
The zinc in long later stage burns, and this compound does not contain heavy metal, and raw material is easy to get, preparation process is simple, and therefore, having good industry should
With prospect, it is a kind of respond well PVC stabilizer.
Specific embodiment
Below by embodiment, the invention will be further elaborated, but is not limited only to the present embodiment.
Plasticizer used in this patent is dioctyl phthalate.
Dispersant used in this patent is epoxidized soybean oil.
Antioxidant used in this patent is phosphorous acid three (2,4- di-tert-butyl-phenyl) ester.
Embodiment 1:
100 parts of polyvinyl chloride, 1 part of calcium stearate, 1 part of cyanuric acid zinc, 0.5 part of urea pyrimidine zinc and 0.2 antioxidant 1076 are placed in
In high mixer, it is slowly added to 5 parts of epoxidized soybean oils and 50 parts of dioctyl phthalates, mixed at high speed during mixed at high speed
10min, makes the powder of within the chamber uniformly mix, and then the material after mixing is being placed in 160 DEG C of roller temperature, the double roller refining of roll spacing is moulded
Plasticate on machine 5 min, after taking piece, is cut into 2cm × 2cm blockage sample, requires according to GB/T 7141-92 standard, by PVC piece
Packet is placed in ageing oven in order, carries out oven ageing experiment test at 190 ± 1 DEG C, takes out test piece every 10 min, sees
Examine and record the change of test piece colourity, till being continued until that black in test piece, according to ASTM D1925-70 standard, remember
Record its yellowness index, the results are shown in Table 1.
Embodiment 2:
By 100 parts of polyvinyl chloride, 0.5 part of calcium stearate, 1.5 parts of cyanuric acid zincs, 0.5 part of urea pyrimidine zinc and 0.2 part of antioxidant,
It is slowly added to 5 parts of epoxidized soybean oils and 50 parts of dioctyl phthalates, mixed at high speed 10min during mixed at high speed, make
The powder of within the chamber uniformly mixes, and then the material after mixing is being placed in 160 DEG C of roller temperature, the double roller plastic-making device of roll spacing is plasticated
5min, after taking piece, is cut into 2cm × 2cm blockage sample, requires according to GB/T 7141-92 standard, PVC piece is grouped in order
It is placed in ageing oven, at 190 ± 1 DEG C, carries out oven ageing experiment test, take out test piece every 10 min, observe and record examination
The change of piece colourity, till being continued until that black in test piece, according to ASTM D1925-70 standard, records its yellowing and refers to
Number, the results are shown in Table 1.
Embodiment 3:
100 parts of polyvinyl chloride, 2 parts of cyanuric acid zincs, 0.5 part of urea pyrimidine zinc and 0.2 antioxidant 1076 are placed in high mixer and put
In high mixer, it is slowly added to 5 parts of epoxidized soybean oils and 50 parts of dioctyl phthalates during mixed at high speed, mixed at a high speed
Close 10min, so that the powder of within the chamber is uniformly mixed, then the material after mixing is placed in 160 DEG C of roller temperature, the double roller refining of roll spacing
Plasticate on molding machine 5min, after taking piece, is cut into 2cm × 2cm blockage sample, requires according to GB/T 7141-92 standard, by PVC
Piece is grouped in order and is placed in ageing oven, carries out oven ageing experiment test at 190 ± 1 DEG C, takes out test piece every 10 min,
Observe and record the change of test piece colourity, till being continued until that black in test piece, according to ASTM D1925-70 standard,
Record its yellowness index, the results are shown in Table 1.
Comparative example 4:
100 parts of polyvinyl chloride, 1 part of zinc stearate, 1 part of calcium stearate and 0.2 part of antioxidant 1076 are placed in high mixer,
It is slowly added to 5 parts of epoxidized soybean oils and 50 parts of dioctyl phthalates, mixed at high speed 10min during mixed at high speed, make chamber
Indoor powder uniformly mixes, and then the material after mixing is being placed in 160 DEG C of roller temperature, the double roller plastic-making device of roll spacing is plasticated
5min, after taking piece, is cut into 2cm × 2cm blockage sample, requires according to GB/T 7141-92 standard, PVC piece is grouped in order
It is placed in ageing oven, at 190 ± 1 DEG C, carries out oven ageing experiment test, take out test piece every 10 min, observe and record examination
The change of piece colourity, till being continued until that black in test piece, according to ASTM D1925-70 standard, records its yellowing and refers to
Number, the results are shown in Table 1.
The impact to PVC yellowness index for the PVC stabilizer of table 1. different process and species
Time/min | 10 | 20 | 30 | 40 | 50 | 60 | 70 | 80 | 90 | 100 |
Embodiment 1 | 6.18 | 8.94 | 14.56 | 19.65 | 28.94 | 39.45 | 41.75 | 45.23 | 49.25 | 52.34 |
Embodiment 2 | 4.16 | 5.28 | 8.96 | 12.37 | 16.24 | 39.48 | 46.68 | 53.26 | 60.52 | 63.11 |
Embodiment 3 | 5.96 | 7.76 | 12.56 | 16.48 | 20.21 | 29.33 | 40.44 | 49.37 | 55.36 | 58.64 |
Comparative example 4 | 10.56 | 12.34 | 19.56 | 26.35 | 30.65 | 41.32 | 49.74 | 55.36 | 63.66 | 69.25 |
It should be pointed out that above example is only the representational example of the present invention.Obviously, technical scheme does not limit
In above-described embodiment, can also there are many deformation.Those of ordinary skill in the art directly can derive from the disclosure of invention
Or all deformation associated, all it is considered as protection scope of the present invention
The heat endurance of cyanuric acid zinc/urea pyrimidine zinc characterizes:
Characterize the thermal decomposition behavior of cyanuric acid zinc/efficient PVC stabilizer of urea pyrimidine zinc Compositional type, result using thermogravimetric analyzer
As shown in Figure 1.
Brief description:
Fig. 1. the heat endurance of cyanuric acid zinc/efficient PVC stabilizer of urea pyrimidine zinc Compositional type characterizes
As seen from the figure, the efficient PVC stabilizer that cyanuric acid zinc/urea pyrimidine zinc compounds has a little micro- in 25-300 DEG C of temperature range
Little weightlessness, this is to be caused by some the absorption water volatilizations in sample.Find out from ensuing TGA curve trend, from 310 DEG C
Start to decompose, its decomposable process can be divided mainly into two stages.The decomposition of first stage is in 310-490 DEG C of this temperature range
Inside carry out, mainly decompose the carbon monoxide having volatilized three molecules, weight loss is about 15.1% (calculated value is 15.9%).
The weightless of second stage sample 21.3% occurs in 490-800 DEG C of this temperature range, and mainly remaining cyanuric acid is organic
The decomposition volatilization (calculated value is 22.7%) of thing part.The residue that sample finally decomposes remaining 63.4% is that Zn0 is (theoretical
Clearing are worth for 61.4%).From here it can also be seen that, the cyanuric acid zinc above being drawn substantially conforms to actual conditions.The opposing party
Face, the efficient PVC stabilizer that cyanuric acid zinc/urea pyrimidine zinc compounds just starts to decompose from 310 DEG C, can protect in PVC process
It is fixed to keep steady, and meets the primary condition as PVC heat stabilizer.
Claims (5)
1. a kind of cyanuric acid zinc/efficient PVC stabilizer of urea pyrimidine zinc Compositional type preparation and application it is characterised in that its component and
Mass parts are as follows:
80 ~ 90 parts of cyanuric acid zinc
10 ~ 20 parts of urea pyrimidine zinc
2 ~ 5 parts of plasticizer
1 ~ 2 part of dispersant
2 ~ 5 parts of antioxidant.
2. a kind of preparation of cyanuric acid zinc according to claim 1/efficient PVC stabilizer of urea pyrimidine zinc Compositional type with should
With it is characterised in that:Described plasticizer is dioctyl phthalate, di-n-octyl phthalate, phthalic acid fourth benzyl
One or more of ester, di-sec-octyl phthalate, dicyclohexyl phthalate.
3. a kind of preparation of cyanuric acid zinc according to claim 1/efficient PVC stabilizer of urea pyrimidine zinc Compositional type with should
With it is characterised in that:Described dispersant is one or more of epoxidized soybean oil, castor oil, silicone oil.
4. a kind of preparation of cyanuric acid zinc according to claim 1/efficient PVC stabilizer of urea pyrimidine zinc Compositional type with should
With it is characterised in that:Described antioxidant includes β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid positive octadecanol ester, bigcatkin willow
Acid phenenyl ester, phosphorous acid three (2,4- di-tert-butyl-phenyl) ester, one or more of 1010,1076.
5. a kind of preparation and application of cyanuric acid zinc/efficient PVC stabilizer of urea pyrimidine zinc Compositional type are it is characterised in that according to following
Step is carried out:A certain amount of cyanuric acid zinc, urea pyrimidine zinc and antioxidant are placed in the mixing of high mixer high speed, in mixed process
Sequentially add appropriate dispersant and plasticizer, mixed at high speed 10min, so that the powder of within the chamber is uniformly mixed.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108774402A (en) * | 2018-06-27 | 2018-11-09 | 杭州三叶新材料股份有限公司 | A kind of PVC calendered sheets special environment protection zinc-base SY-310 stabilizer synthetic methods |
CN108997672A (en) * | 2018-06-27 | 2018-12-14 | 杭州三叶新材料股份有限公司 | A kind of zinc-base stabilizer and preparation method thereof applied to transparent calendared sheet |
WO2020248381A1 (en) * | 2019-06-13 | 2020-12-17 | 深圳市志海实业股份有限公司 | Method for solid-phase synthesis of cyanuric acid-uracil complex zinc salt |
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CN103183644A (en) * | 2011-12-31 | 2013-07-03 | 深圳市志海实业有限公司 | Uracil zinc salt and application thereof as heat stabilizer for PVC |
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CN103183644A (en) * | 2011-12-31 | 2013-07-03 | 深圳市志海实业有限公司 | Uracil zinc salt and application thereof as heat stabilizer for PVC |
CN104877179A (en) * | 2015-03-31 | 2015-09-02 | 杭州鸿雁管道系统科技有限公司 | Organic composite heat stabilizer and preparation method thereof |
Non-Patent Citations (1)
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108774402A (en) * | 2018-06-27 | 2018-11-09 | 杭州三叶新材料股份有限公司 | A kind of PVC calendered sheets special environment protection zinc-base SY-310 stabilizer synthetic methods |
CN108997672A (en) * | 2018-06-27 | 2018-12-14 | 杭州三叶新材料股份有限公司 | A kind of zinc-base stabilizer and preparation method thereof applied to transparent calendared sheet |
WO2020248381A1 (en) * | 2019-06-13 | 2020-12-17 | 深圳市志海实业股份有限公司 | Method for solid-phase synthesis of cyanuric acid-uracil complex zinc salt |
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Application publication date: 20170222 |