CN106221072A - A kind of asepsis environment-protecting stabilizer being used in high PVC product thoroughly and production method thereof - Google Patents
A kind of asepsis environment-protecting stabilizer being used in high PVC product thoroughly and production method thereof Download PDFInfo
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- CN106221072A CN106221072A CN201610704914.5A CN201610704914A CN106221072A CN 106221072 A CN106221072 A CN 106221072A CN 201610704914 A CN201610704914 A CN 201610704914A CN 106221072 A CN106221072 A CN 106221072A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
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- 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
Abstract
The invention discloses a kind of asepsis environment-protecting stabilizer being used in high PVC product thoroughly and production method thereof.This stabilizer is consisted of by mass fraction: the polrvinyl chloride (PVC) of 100 parts, the calcium zincates of 24 parts, the sodium stearate of 0.06 0.12 parts.Its action principle is that calcium zincates contains great amount of hydroxy group, it is possible to neutralize the HCl that a large amount of PVC degraded is discharged, and the metallic element environmentally safe such as zinc, calcium.So that PVC stabilizer prepared by the method substitutes traditional stabilizer, production method is simple, low cost, environmentally safe.It is expected to substitute traditional stabilizer and becomes novel PVC stabilizer nontoxic, cheap, efficient.
Description
Technical field
The present invention uses water-bath crystallization method to synthesize calcium zincates, uses sodium stearate to carry out wet-process modified to calcium zincates.Modified
After calcium zincates and calcium stearate compound in proportion.
Background technology
Polrvinyl chloride [poly (vinyl choride), PVC] is one of five big synthetic resin that consumption is maximum in the world,
It it is the thermoplastic linear's polymer generated through Raolical polymerizable by Vinyl Chloride Monomer.It is low that PVC material has high intensity, price
Honest and clean, chemical resistance is good, electrical insulating property is good and the advantage such as difficult to burn, and is easily worked, and can pass through mold pressing, lamination, note
The various ways such as mould to be processed, be widely used in engineering construction, the hard of packaging for foodstuff, the industry such as electrically and soft goods.With
Further expanding of application, continuation is increased by the demand of PVC.
Although PVC has superior performance, but owing to PVC polymer chain structure containing branch point, double bond and initiator
The existence of the unstable factors such as residue so that the chlorosity on PVC strand is easily deviate from from strand, when being heated to 140 DEG C just
Can decompose and discharge hydrogen chloride.Along with extending heating time or temperature raise, HCL deviates from a large number and accumulates in the material, by
In HCL, PVC degraded is had catalytic action so that PVC degradation speed greatly speeds up, after abjection HCL, strand is formed in a large number
Having the conjugated double bond added lustre to, goods occur that color is drastically deepened, and the phenomenon that physical and mechanical properties declines, even carbonization are until losing
Raw use value.Therefore, it is shaped adding man-hour in PVC product, it is necessary to use heat stabilizer.
The thirties in 20th century, first the appearance of lead salt solves the thermal degradation problems of PVC, is also use the earliest thermally-stabilised
Agent, but along with the enhancing of people's environmental consciousness, its toxicity problem big, with serious pollution significantly limit application；The most gradually
Create metallic soap, organotin, rare earth and a large amount of auxiliary heat stabilizers etc..Along with many Environmental protective awareness in the world
Raising and environmental problem increasingly serious, the health problem about people's daily life is paid close attention to by everybody.PVC product conduct
Use face general-purpose plastics the most widely, in tradition PVC product as the face of use general-purpose plastics the most widely, at tradition PVC
Heat stabilizer in, owing to the heat stabilizer containing heavy metal such as lead salts has good superiority of effectiveness, once by human body
Just cannot excrete after absorption, have a strong impact on the health of direct labor；Contain the PVC product of lead salt in use simultaneously
Being separated out as well as extending with of time, this also has influence on the healthy of user, particularly medical and health, child
Toy and the product relevant to packaging for foodstuff are particularly acute.Therefore, the tradition poisonous heat stabilizer containing heavy metal will be by entirely
Face replaces, and this type thermal stabilizing agent will certainly step down from the stage of history.The Non-toxic direction of following PVC heat stabilizer is concentrated mainly on
Calcium/zinc composite heat stabilizer and organotin two aspect.Organo-tin het stabilizer has the heat stability of excellence, but its price is held high
Expensive, limit it and use popularization；And Ca/Zn complex stabilizer is universally acknowledged non-toxic plastic product additive, Ca/Zn is compound steady
Determine the main body that agent will finally build the PVC stabilizer system of various countries in future due to excellent combination property and high performance-price ratio.
Calcium zincates is laminated structure, containing great amount of hydroxy group, it is possible to neutralize the HCL that substantial amounts of PVC thermal degradation process is discharged.
And zinc contained in calcium zincates, calcium, etc. metallic element PVC is had to certain heat stabilization.Hydrocalumite is
A kind of Layered compound, has the layer structure of houghite, and interlayer may be inserted into various the moon to PVC with heat stabilization
Ion.And calcium zincates and water aluminum calcium are readily synthesized, cost is relatively low, environmentally safe.
Summary of the invention
It is an object of the invention to combine existing technology, it is provided that a kind of new method synthesis calcium zincates, use stearic acid
Sodium carries out surface modification to calcium zincates, and calcium zincates is modified to be compounded in proportion with calcium stearate.And make PVC with the addition of this
Composite processing performance and thermal stability that kind heat stabilizer obtains all have stable lifting.It is a kind of workable, raw
Product method is simple, environmentally safe, the effective ways that cost price is low.
To achieve these goals, technical solution of the present invention is as follows: a kind of asepsis environment-protecting being used in high PVC product thoroughly is steady
Determine agent and production method thereof, under its constituent and mass fraction are.
Calcium hydroxide 0.6-1.2 part
Zinc oxide 1.4-2.8 part
Sodium stearate 0.06-0.12 part
Calcium stearate 1-2 part
Wherein said calcium hydroxide purity is AR
Wherein said purity zinc oxide is AR
Wherein said sodium stearate purity is CP
Wherein said calcium stearate purity is AR
(1) weigh calcium hydroxide and zinc oxide by the amount of material respectively than for 1:2.02, be placed in reactor.Add in reactor
Enter excess deionized water, control reaction temperature at 70-100 DEG C.
(2) continuously stirred, successive reaction 12h, obtain milk-white coloured suspension after stopped reaction, suspension is quiet as room temperature
Put ageing 12h, make product crystal growth.Product after removing supernatant rinses to neutral and sucking filtration, is placed in by filter cake
The vacuum drying oven of 60 DEG C is dried and is ground, obtain the solid calcium zincates sample of preparation.
(3) solid calcium zincates sample is placed in beaker, adds deionized water, add the stearic acid accounting for sample quality 3%
Sodium.Beaker is placed in water-bath, continuous stirring stoichiometric number hour.Precipitate obtained by previous step is carried out sucking filtration, washing,
Being neutrality to filtrate.Filter cake is placed in 60 DEG C of vacuum drying ovens and is dried, after being dried, i.e. obtain modified zincic acid
Calcium sample.
(4) modified calcium zincates sample and stearic acid are compounded in proportion carry out in homogenizer, after completing i.e.
Obtain compound calcium zincates heat stabilizer.
Above-mentioned a kind of asepsis environment-protecting stabilizer being used in high PVC product thoroughly and production method thereof, its feature is prepared
Calcium zincates stabilizer is compared with general zinc soap type thermal stabilizing agent, due to Ca2+Existence, can with in PVC ageing process produce
ZnCl2React, regenerate Zn2+And the CaCl remained2To PVC non-hazardous, thus i.e. can be to a certain extent
Suppression zinc burn so that the long-time stability of PVC relative to general zinc-base stabilizer to certain improvement.
The invention have the benefit that preparation technology is simple, low cost.The stability simultaneously making PVC has obtained very
Good improvement.
Detailed description of the invention
Calcium hydroxide of the present invention is characterized in that its purity is AR.
Wherein said zinc oxide is characterized in that its purity is AR.
Wherein said sodium stearate is as the modifying agent of stabilizer, and its purity is CP.
Wherein said calcium stearate is as improving initial stage thermostable effect and can suppress the auxiliary heat of " zinc burning " surely
Determine the compounding use of agent, it is characterised in that its purity is AR.
Wherein said polrvinyl chloride is that the degree of polymerization is relatively low such as, molecular weight 5W ~ 11W, and the degree of polymerization is 800, and the degree of polymerization is relatively
The PVC that the trade mark is S-700 that low easy processing, such as Changzhou curry favour profit trade Co., Ltd provide.
A kind of asepsis environment-protecting stabilizer being used in high PVC product thoroughly
(1) weigh calcium hydroxide and zinc oxide by the amount of material respectively than for 1:2.02, prepare solid zincic acid by water-bath crystallization method
Calcium.
(2) solid calcium zincates sample is placed in beaker, adds deionized water, add the stearic acid accounting for sample quality 3%
Sodium.Calcium zincates sample has been carried out wet-process modified.
(3) pulverize and sieve with pulverizer again obtain be modified calcium zincates stabilizer.
(4) modified calcium zincates sample and stearic acid are compounded in proportion carry out in homogenizer, after completing i.e.
Obtain compound calcium zincates heat stabilizer.
A kind of asepsis environment-protecting stabilizer being used in high PVC product thoroughly and production method thereof, its feature is prepared
Calcium zincates stabilizer is compared with general zinc soap type thermal stabilizing agent, due to Ca2+Existence, can with in PVC ageing process produce
ZnCl2React, regenerate Zn2+And the CaCl remained2To PVC non-hazardous, thus i.e. can be to a certain extent
Suppression zinc burn so that the long-time stability of PVC relative to general zinc-base stabilizer to certain improvement.Calcium stearate with contain
Zn heat stabilizer used time, can effectively replace the unstable chlorine atom in PVC under Zn2+ is catalyzed, make up lacking of PVC
Fall into structure, stop alkene structures growth, effectively inhibit its initial coloration.
Embodiment 1
Formula: polrvinyl chloride 100 parts, calcium zincates 2 parts, sodium stearate 0.06 part, calcium stearate 2 parts
Solid calcium zincates sample is placed in beaker, adds deionized water, add the sodium stearate of 0.12 part.Beaker is placed in
In water-bath, continuous stirring stoichiometric number hour.Precipitate obtained by previous step is carried out sucking filtration, washing, is neutrality to filtrate
Till.Filter cake is placed in 60 DEG C of vacuum drying ovens and is dried, after being dried, i.e. obtain modified calcium zincates sample.By modification
After calcium zincates sample and stearic acid compound in proportion and carry out in homogenizer, i.e. obtain compound calcium zincates heat after completing steady
Determine agent.Again by proportioning by polrvinyl chloride and compound after calcium zincates heat stabilizer stabilizer use homogenizer to mix,
Obtain poly (vinyl chloride) blend.Polyethylene mixture is placed in two-roll mill, at 195 DEG C of mixing 5min, makes 1mm thickness
Thin slice, shreds thin slice after cooling and becomes the little granule of the length of side about 1mm, be placed in test tube, the most about 5cm.Test tube is dipped in 195
DEG C oil bath pan in, make sample surfaces in test tube be in same horizontal line with the pasta in oil bath pan.Record is from test tube
Immersing oil bath pan to start until becoming, shortly past red reagent paper color, the time that indigo plant is experienced, this is heat-stable time, in units of min
Represent.Each sample is carried out three Congo red tests, averages.Measurement result such as table one.
Embodiment 2
Formula: polrvinyl chloride 100 parts, calcium zincates 3 parts, sodium stearate 0.09 part, calcium stearate 2 parts
Solid calcium zincates sample is placed in beaker, adds deionized water, add the sodium stearate of 0.09 part.Beaker is placed in
In water-bath, continuous stirring stoichiometric number hour.Precipitate obtained by previous step is carried out sucking filtration, washing, is neutrality to filtrate
Till.Filter cake is placed in 60 DEG C of vacuum drying ovens and is dried, after being dried, i.e. obtain modified calcium zincates sample.By modification
After calcium zincates sample and stearic acid compound in proportion and carry out in homogenizer, i.e. obtain compound calcium zincates heat after completing steady
Determine agent.Again by proportioning by polrvinyl chloride and compound after calcium zincates stabilizer use homogenizer to mix, obtain polychlorostyrene
Mixture of ethylene.Polyethylene mixture is placed in two-roll mill, at 195 DEG C of mixing 5min, makes the thick thin slice of 1mm, cold
The most afterwards thin slice is shredded and become the little granule of the length of side about 1mm, be placed in test tube, the most about 5cm.Test tube is dipped in the oil of 195 DEG C
In bath, the sample surfaces in test tube is made to be in same horizontal line with the pasta in oil bath pan.Record and immerse oil from test tube
Bath starts until becoming, shortly past red reagent paper color, the time that indigo plant is experienced, and this is heat-stable time, represents in units of min.
Each sample is carried out three Congo red tests, averages.Measurement result such as table one.
Formula: polrvinyl chloride 100 parts, calcium zincates 3 parts, sodium stearate 0.12 part, calcium stearate 2 parts
Solid calcium zincates sample is placed in beaker, adds deionized water, add the sodium stearate of 0.12 part.Beaker is placed in
In water-bath, continuous stirring stoichiometric number hour.Precipitate obtained by previous step is carried out sucking filtration, washing, is neutrality to filtrate
Till.Filter cake is placed in 60 DEG C of vacuum drying ovens and is dried, after being dried, i.e. obtain modified calcium zincates sample.By modification
After calcium zincates sample and stearic acid compound in proportion and carry out in homogenizer, i.e. obtain compound calcium zincates heat after completing steady
Determine agent.Again by proportioning by polrvinyl chloride and compound after calcium zincates stabilizer use homogenizer to mix, obtain polychlorostyrene
Mixture of ethylene.Polyethylene mixture is placed in two-roll mill, at 195 DEG C of mixing 5min, makes the thick thin slice of 1mm, cold
The most afterwards thin slice is shredded and become the little granule of the length of side about 1mm, be placed in test tube, the most about 5cm.Test tube is dipped in the oil of 195 DEG C
In bath, the sample surfaces in test tube is made to be in same horizontal line with the pasta in oil bath pan.Record and immerse oil from test tube
Bath starts until becoming, shortly past red reagent paper color, the time that indigo plant is experienced, and this is heat-stable time, represents in units of min.
Each sample is carried out three Congo red tests, averages.Measurement result such as table one.
Comparative example 1
Formula: polrvinyl chloride 100 parts
Polyethylene is placed in two-roll mill, at 195 DEG C of mixing 5min, makes the thick thin slice of 1mm, after cooling, thin slice is shredded
Become the little granule of the length of side about 1mm, be placed in test tube, the most about 5cm.Test tube is dipped in the oil bath pan of 195 DEG C, makes in test tube
Sample surfaces and oil bath pan in pasta be in same horizontal line.Record from test tube immerse oil bath pan start until shortly past
Red reagent paper color becomes the time that indigo plant is experienced, and this is heat-stable time, represents in units of min.Each sample is carried out three
Secondary Congo red is tested, and averages.Measurement result such as table one.
Comparative example 2
Formula: polrvinyl chloride 100 parts, calcium zincates 2 parts, calcium stearate 2 parts
Unmodified calcium zincates sample and stearic acid are compounded in proportion and carries out in homogenizer, be i.e. combined after completing
Calcium zincates heat stabilizer.By polrvinyl chloride and compound after calcium zincates stabilizer homogenizer mix, obtain polychlorostyrene
Mixture of ethylene.Polyethylene mixture is placed in two-roll mill, at 195 DEG C of mixing 5min, makes the thick thin slice of 1mm, cold
The most afterwards thin slice is shredded and become the little granule of the length of side about 1mm, be placed in test tube, the most about 5cm.Test tube is dipped in the oil of 195 DEG C
In bath, the sample surfaces in test tube is made to be in same horizontal line with the pasta in oil bath pan.Record and immerse oil from test tube
Bath starts until becoming, shortly past red reagent paper color, the time that indigo plant is experienced, and this is heat-stable time, represents in units of min.
Each sample is carried out three Congo red tests, averages.Measurement result such as table one.
Comparative example 3
Formula: polrvinyl chloride 100 parts, calcium zincates 3 parts, calcium stearate 2 parts
Unmodified calcium zincates sample and stearic acid are compounded in proportion and carries out in homogenizer, be i.e. combined after completing
Calcium zincates heat stabilizer.By polrvinyl chloride and compound after calcium zincates stabilizer homogenizer mix, obtain polychlorostyrene
Mixture of ethylene.Polyethylene mixture is placed in two-roll mill, at 195 DEG C of mixing 5min, makes the thick thin slice of 1mm, cold
The most afterwards thin slice is shredded and become the little granule of the length of side about 1mm, be placed in test tube, the most about 5cm.Test tube is dipped in the oil of 195 DEG C
In bath, the sample surfaces in test tube is made to be in same horizontal line with the pasta in oil bath pan.Record and immerse oil from test tube
Bath starts until becoming, shortly past red reagent paper color, the time that indigo plant is experienced, and this is heat-stable time, represents in units of min.
Each sample is carried out three Congo red tests, averages.Measurement result such as table one.
Comparative example 4
Formula: polrvinyl chloride 100 parts, calcium zincates 4 parts, calcium stearate 2 parts
Unmodified calcium zincates sample and stearic acid are compounded in proportion and carries out in homogenizer, be i.e. combined after completing
Calcium zincates heat stabilizer.By polrvinyl chloride and compound after calcium zincates stabilizer homogenizer mix, obtain polychlorostyrene
Mixture of ethylene.Polyethylene mixture is placed in two-roll mill, at 195 DEG C of mixing 5min, makes the thick thin slice of 1mm, cold
The most afterwards thin slice is shredded and become the little granule of the length of side about 1mm, be placed in test tube, the most about 5cm.Test tube is dipped in the oil of 195 DEG C
In bath, the sample surfaces in test tube is made to be in same horizontal line with the pasta in oil bath pan.Record and immerse oil from test tube
Bath starts until becoming, shortly past red reagent paper color, the time that indigo plant is experienced, and this is heat-stable time, represents in units of min.
Each sample is carried out three Congo red tests, averages.Measurement result such as table one.
The present invention as can be seen from the above table.So that PVC stabilizer prepared by the method substitutes traditional stabilizer, production method
Simply, low cost, environmentally safe.It is expected to substitute traditional stabilizer and becomes novel PVC nontoxic, cheap, efficient stably
Agent.
Claims (3)
1. the asepsis environment-protecting stabilizer being used in high PVC product thoroughly and production method thereof, it is characterised in that: described hydroxide
Calcium and zinc oxide synthesis calcium zincates are made up of the component of following mass fraction
Calcium hydroxide 0.6-1.2 part
Zinc oxide 1.4-2.8 part
Sodium stearate 0.06-0.12 part
Calcium stearate 1-2 part
Wherein said calcium hydroxide is characterized in that its purity is AR；
Wherein said zinc oxide is characterized in that its purity is AR；
Wherein said sodium stearate is as the modifying agent of stabilizer, and its purity is CP；
Wherein said calcium stearate is as improving initial stage thermostable effect and can suppress the auxiliary heat stabilizer of " zinc burning "
Compounding use, it is characterised in that its purity is AR.
2. the asepsis environment-protecting stabilizer being used in high PVC product thoroughly, it is characterised in that prepare as steps described below
(1) weigh calcium hydroxide and zinc oxide by the amount of material respectively than for 1:2.02, be placed in reactor；Add in reactor
Enter excess deionized water, control reaction temperature at 70-100 DEG C；
(2) continuously stirred, successive reaction 12h, obtain milk-white coloured suspension after stopped reaction, suspension is stood old as room temperature
Change 12h, make product crystal growth；Product after removing supernatant rinses to neutral and sucking filtration, and filter cake is placed in 60 DEG C
Vacuum drying oven in be dried be ground, obtain preparation solid calcium zincates sample；
(3) solid calcium zincates sample is placed in beaker, adds deionized water, add the sodium stearate accounting for sample quality 3%；
Beaker is placed in water-bath, continuous stirring stoichiometric number hour；Precipitate obtained by previous step is carried out sucking filtration, washing, extremely
Till filtrate is neutrality；Filter cake is placed in 60 DEG C of vacuum drying ovens and is dried, after being dried, i.e. obtain modified calcium zincates
Sample；
(4) modified calcium zincates sample and stearic acid are compounded in proportion carry out in homogenizer, i.e. obtain after completing
Compound calcium zincates heat stabilizer.
3. being used in the asepsis environment-protecting stabilizer in high PVC product thoroughly and a production method thereof, its feature is prepared zinc
Acid calcium stable agent is compared with general zinc soap type thermal stabilizing agent, due to Ca2+Existence, can with in PVC ageing process produce
ZnCl2React, regenerate Zn2+And the CaCl remained2To PVC non-hazardous, thus i.e. can press down to a certain extent
Zinc processed burn so that the long-time stability of PVC relative to general zinc-base stabilizer to certain improvement.
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2016
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| CN101235162A (en) * | 2008-03-04 | 2008-08-06 | 四川大学 | Method for preparing granulating auxiliary agent for processing plastic |
| DE102008053629A1 (en) * | 2008-10-29 | 2010-05-12 | Baerlocher Gmbh | Stabilizer composition, useful for stabilizing halogen containing polymers, comprises glycerol monoalkyl-ethers and organic or inorganic compound containing di- or tri- or tetravalent metal capable of forming salts with mineral acid |
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Application publication date: 20161214 |