CN102675774A - PVC (polyvinyl chloride) composite material modified foaming agent, micro foaming PVC composite material and preparation method thereof - Google Patents
PVC (polyvinyl chloride) composite material modified foaming agent, micro foaming PVC composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a PVC (polyvinyl chloride) composite material modified foaming agent, a micro foaming PVC composite material and a preparation method thereof. The method comprises the following steps: PVC is adopted as a raw material; foaming agent, ultra-fine active calcium carbonate, plasticizer, heat stabilizer and anti-oxidant are added; and the ingredients are mixed simply in a high speed mixer, plasticized through an internal mixer, plasticated in a double-roller open type plasticating machine, calendered and formed though a four-roller plastic calender after being combined with base fabric, and then foamed and formed by a foaming stove, so as to obtain the micro foaming PVC composite material with compact, uniform and smaller bubble holes. The invention has the advantages that the bubble holes of the PVC composite material prepared according the method are high in density, small in size and uniform in distribution; the consumption of the foaming agent is reduced; the PVC plasticization temperature region is enlarged; the production cost is reduced; the ageing-resistance is excellent; and the mechanical property is favorable.
Description
Technical field
The invention belongs to the polymer material science field, be specifically related to the preparation of PVC matrix material.
Technical background
Along with present science and technology development; People are also increasingly high to the requirement of quality of life, and leatheroid enters in people's the family life gradually, and are widely used in fields such as sofa fabric, automotive trim, case and bag footwear; PVC is a kind of as leatheroid; Rely on its less cost, abundant source is the object that people study always, and the range of application for enlarging PVC improves its performance and quality and has important effect.
Patent publication No. is CN101838937A disclosed " a kind of ecological PVC decorative artificial leather and preparation method thereof "; Utilize the PVC slurry to make through rolling process; This patent is made softening agent with epoxy soybean oil; Preferably resolve problem of environmental pollution, and finished product has the degree of folding labor preferably, matrix material has certain mechanical property.Number of patent application is CN102002865A disclosed " high-elastic PVC synthetic leather and a working method thereof "; Utilize PVC as resin matrix; Make leatheroid through adding whipping agent, filler etc., yet because the existence of DOP there is certain influence to environment than higher gears.
But above-mentioned two parts of patents all do not solve the fine and close problem of abscess, and the defective of bringing is: subsiding and breaking of abscess makes the mechanical property of PVC matrix material and quality be not so good as people's will.
The production technology of PVC leatheroid is comparatively ripe; Along with the performance requriements to synthetic leather is increasingly high; Further optimize the component of PVC matrix material; The PVC artificial leather material matrix of development of new seems particularly important, for the research of the little foaming technique of PVC matrix material, carries out as far as possible and the keeping in of environment; Optimizing design of components has become and has enlarged PVC leatheroid range of application important factor, obtains that mechanical property is good, abscess-size is less and abscess is fine and close, reduces subsiding and break and having important effect for the quality that improves the PVC leatheroid of abscess.
Summary of the invention
The present invention aims to provide a kind of PVC composite modification whipping agent, simultaneously little foaming PVC matrix material with this whipping agent is provided; The little foaming PVC matrix material abscess-size that obtains is little and abscess is fine and close; Can improve the mechanical property and the quality of PVC micro-foaming material; Overcome subsiding and breaking of abscess in the prior art, help the further development and application of PVC leatheroid.The present invention will provide the preparation method of little foaming PVC matrix material simultaneously.
The present invention realizes through following technical scheme:
PVC composite modification whipping agent, form by the raw material of following weight part:
1～5 part of whipping agent Cellmic C 121,2～5 parts of dispersion agents, foam stabilizer 0.5-2 part, Zinic stearas and zinc oxide proportioning are 0.5～1 part of compound, 0.1～2 part in the oxidation inhibitor of 2-5:1;
Above-mentioned raw materials is added in the mixing machine by said weight part, under 60～80 ℃ of conditions, mix 15～20min.The mixing machine rotating speed is at 750-1500r/min.
The further improvement project of the present invention is that said dispersion agent is to be to be formed according to the ratio of 1:1～5 is composite by whiteruss and Tristearoylglycerol.
The further improvement project of the present invention is, foam stabilizer is YSR 3286-polyoxy alkylene segmented copolymer, gather one or both mixtures in the methyl silicon SULPHOSUCCINIC ACID ESTER.
The further improvement project of the present invention is; Oxidation inhibitor is four [β-(3; The 5-di-tert-butyl-hydroxy phenyl) propionic acid] one or more mixtures in pentaerythritol ester, three ［ 2.4-di-tert-butyl-phenyl ］ phosphorous acid ester, β-positive octadecanol ester of (3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid.
Said modified foaming agent gas forming amount is 210-215ml/g, at 0-185 ℃ of Heat stability is good, rate of decomposition＜1%.
Little foaming PVC matrix material; Raw material by following weight part; Through mixing, fusion plastification, foaming: 40～80 parts of SE (polymerization degree is 1000-2000), 1～5 part of above-mentioned modified foaming agent, 20～60 parts of superfine active calcium carbonates; 10～40 parts in softening agent, 0.5～5 part of thermo-stabilizer.
The further improvement project of the present invention is that said superfine active calcium carbonate is the 1250-2500 order.
The further improvement project of the present invention is that softening agent is one or both mixtures in Witcizer 300, the tributyl citrate.
The further improvement project of the present invention is that said thermo-stabilizer is one or more mixtures in barium zinc composite stabilizer, thiol methyl tin, the antimony organic thermo-stabilizer.
Prepare the method for above-mentioned little foaming PVC matrix material, may further comprise the steps:
(1) mixing of materials: by above-mentioned proportioning, with SE, modified foaming agent, superfine active calcium carbonate, softening agent, thermo-stabilizer add in the mixing machine, are under the 70-90 ℃ of condition in the material temperature, mixed at high speed 15-25min;
(2) fusion plastification: the material of step (1) gained is plastified in Banbury mixer, and plasticization temperature is 130-150 ℃, and fusion time is 3-5min; Material with gained is transferred to further fusion plastification in two roller open mills then; Plasticization temperature is 140-160 ℃, and fusion time is 5-10min, will plastify then good material through travelling belt move in the four roller plastic calenders fit with base cloth after; The first and second roller temperature controls are at 165-175 ℃; The third and fourth roller temperature control is between 110-130 ℃, and roller speed is 30-45Hz/min, and traction is batched and obtained work in-process then;
(3) foaming: step (2) gained work in-process through the cylinder traction, are imported foaming furnace, and the mold temperature in the foaming furnace is between 180-210 ℃; Foamed time is 1-2min; After polyvinyl chloride resin leaves foaming furnace air cooling 3-5s, roll stamp again and handle, batch the acquisition finished product.
The present invention compared with prior art has the following advantages:
One, select superfine active calcium carbonate, realized the good binding of lime carbonate and resin, the existence of dispersion agent simultaneously makes treated carbonates dispersed better in resin, help abscess formation homogeneity, density compactness.
Two, because whipping agent of the present invention is the whipping agent behind the modified active; Reduced the decomposition temperature of whipping agent; Simultaneously do not influence the thermostability under the whipping agent low temperature, help plasticating fully under the coldcondition, enable in calender line, to be decomposed to form smoothly and faster abscess; Foam structure is comparatively stable, and the situation of subsiding significantly improves.
Three, the present invention adopts the environment-friendly type softening agent, and asepsis environment-protecting has the satisfactory stability effect to light and heat; Reduce the plasticization temperature of PVC; Increased the shaping plasticized temperature range of PVC, high-temperature stability is preferably arranged, alternative o-phthalic acid dibutyl ester etc. are to the influential chemical plasticizing agent of environment.
Four, the present invention has improved the decomposition temperature of PVC owing to added thermo-stabilizer, and nontoxic, no flying dust and can improve the speed of whipping agent decomposition has reduced the volatilization of softening agent, lower melting point auxiliary agent.
Description of drawings
Fig. 1 is the Electronic Speculum figure (can intuitively show structure and size that bubble is empty) of the embodiment of the invention 1 prepared sample.
Fig. 2 is the Electronic Speculum figure of the embodiment of the invention 2 prepared samples.
Accompanying drawing 3 is the Electronic Speculum figure of the embodiment of the invention 3 prepared samples.
Embodiment
Embodiment 1.
The preparation of modified foaming agent: get 2 parts of Cellmic C 121s, 2 parts of dispersion agents, gather methyl silicon phosphoesterase 30 .5 part, Zinic stearas and 0.5 part of zinc oxide (proportioning is 3/1) compound, four [β-(3; The 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester mixes 15～20min for 0.5 part in high-speed mixer; The material temperature is 60～80 ℃, makes modified foaming agent, and the modified foaming agent gas forming amount is 210ml/g; At 0-180 ℃ of Heat stability is good, rate of decomposition＜1%.The dispersion agent that adopts in the present embodiment is formed according to the ratio of 1:1 is composite by whiteruss and Tristearoylglycerol.
The preparation of little foaming PVC matrix material:
Get 50 parts of SE (polymerization degree is 1500); 3 parts of above-mentioned modified foaming agents; 40 parts of superfine active calcium carbonates (1250 order), 10 parts of Witcizer 300s, thiol methyl tin mixes 15-25min for 0.5 part in high-speed mixer; The material temperature is 70-90 ℃, and the material that obtains mixing is subsequent use.
The PVC fusion plastification: above-mentioned material is plastified in Banbury mixer, and plasticization temperature is 140 ℃, and fusion time is 5min; Material with gained is transferred to further fusion plastification in two roller open mills then; Plasticization temperature is 145 ℃, and fusion time is 5min, and then will plastify good material and move to through travelling belt and fit with base cloth in the four roller plastic calenders; First and second roll temperatures are 170 ℃; Third and fourth roll temperature be 110 ℃ it, roller speed is 35Hz/min, traction is batched and is obtained work in-process then.
PVC foaming: above-mentioned work in-process through the cylinder traction, are imported foaming furnace, it is foamed in foaming furnace; Mold temperature is controlled at 185 ℃, and foamed time is 1.5min, introduces the ventilation retrieving arrangement simultaneously; Make the hot gas flow of generation further cool off recycling, guarantee that barometric point and the ambient pressure in the stove remains basically stable, then after the polyvinyl chloride resin product leaves foaming furnace air cooling 3s with the softening agent that volatilizes; Roll stamp again and handle, batch and obtain little foaming PVC matrix material.
Shown in accompanying drawing 1, little foaming PVC matrix material abscess evenly and not subsides, and abscess-size is 110-150 μ m, and density is 0.69g/cm
3
Little foaming PVC performance of composites is following:
Warp tensile strength 7.6MPa has improved 8.2% than existing technology, and weft tensile strength 7.4MPa has improved 7.6% than prior art, peel load 30N.
Embodiment 2.
The preparation of modified foaming agent: get 0.5 part of compound of 3 parts of Cellmic C 121s, 3 parts of dispersion agents, 1 part of foam stabilizer, Zinic stearas and zinc oxide (proportioning is 2/1), oxidation inhibitor mixes 15～20min for 0.5 part in high-speed mixer; The material temperature is 60～80 ℃; Make modified foaming agent; The modified foaming agent gas forming amount is 215ml/g, at 0-185 ℃ of Heat stability is good, rate of decomposition＜1%.The dispersion agent that adopts in the present embodiment is formed according to the ratio of 1:2 is composite by whiteruss and Tristearoylglycerol.Foam stabilizer is YSR 3286-polyoxy alkylene segmented copolymer, and what oxidation inhibitor adopted is three ［ 2.4-di-tert-butyl-phenyl ］ phosphorous acid ester.
The preparation of little foaming PVC matrix material:
Get 40 parts of SE (polymerization degree is 2000), 4 parts of above-mentioned modified foaming agents, 40 parts of superfine active calcium carbonates (2000 order); 15 parts of tributyl citrates; The barium zinc composite stabilizer mixes 15-25min for 0.5 part in high-speed mixer, the material temperature is 70-90 ℃, the material that obtains mixing.
The PVC fusion plastification: the material of gained is plastified in Banbury mixer, and plasticization temperature is 150 ℃, and fusion time is 3min; Material with gained is transferred to further fusion plastification in two roller open mills then; Plasticization temperature is 160 ℃, and fusion time is 5min, and then will plastify good material and move to through travelling belt and fit with base cloth in the four roller plastic calenders; First and second roll temperatures are 175 ℃; Third and fourth roll temperature is 120 ℃, and roller speed is 30Hz/min, and traction is batched and obtained work in-process then.
PVC foaming: resulting work in-process through the cylinder traction, are imported foaming furnace, it is foamed in foaming furnace; Mold temperature is controlled between 190 ℃; Foamed time is 1min, introduces the ventilation retrieving arrangement simultaneously, makes the hot gas flow of generation and the softening agent that volatilizes further cool off recycling; Guarantee that barometric point and ambient pressure in the stove remain basically stable; After the polyvinyl chloride resin product leaves foaming furnace air cooling 3s, roll stamp again and handle then, batch and obtain little foaming PVC matrix material.
Shown in accompanying drawing 2, little foaming PVC matrix material abscess evenly and not subsides, and abscess-size is 110-130 μ m, and density is 0.67g/cm
3
The PVC performance of composites is following:
Radial drawing intensity 8.2MPa has improved 16.8% than existing technology; Weft tensile strength 7.4MPa has improved 7.6% than prior art, peel load 32N.
Embodiment 3.
The preparation of modified foaming agent: get 0.5 part of compound of 4 parts of Cellmic C 121s, 3 parts of dispersion agents, 1 part of foam stabilizer, Zinic stearas and zinc oxide (proportioning is 4/1), oxidation inhibitor mixes 15～20min for 0.5 part in high-speed mixer; The material temperature is 60～80 ℃; Make modified foaming agent; The modified foaming agent gas forming amount is 214ml/g, at 0-180 ℃ of Heat stability is good, rate of decomposition＜0.5%.The dispersion agent that adopts in the present embodiment is formed according to the ratio of 1:4 is composite by whiteruss and Tristearoylglycerol; Foam stabilizer is to gather methyl silicon SULPHOSUCCINIC ACID ESTER and gather methyl silicon phosphate mixture (mixing by 1:1); Oxidation inhibitor is four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester and three ［ 2.4-di-tert-butyl-phenyl ］ phosphite mixture (mixing by 1:1).
The preparation of little foaming PVC matrix material:
With 50 parts of SE (polymerization degree is 1800); 4 parts of modified foaming agents, 35 parts of superfine active calcium carbonates (2500 order), Witcizer 300 and 15 parts in tributyl citrate mixture (mixing) by 1:1; Barium zinc composite stabilizer and 0.5 part of thiol methyl tin mixture (mixing) by 1:1; In high-speed mixer, mix 15-25min, the material temperature is 70-90 ℃, the material that obtains mixing.
The PVC fusion plastification: the material of gained is plastified in Banbury mixer, and plasticization temperature is 145 ℃, and fusion time is 3min; Material with gained is transferred to further fusion plastification in two roller open mills then; Plasticization temperature is 150 ℃, and fusion time is 5min, and then will plastify good material and move to through travelling belt and fit with base cloth in the four roller plastic calenders; First and second roll temperatures are 180 ℃; Third and fourth roll temperature is 120 ℃, and roller speed is 32Hz/min, and traction is batched and obtained work in-process then.
PVC foaming: resulting work in-process through the cylinder traction, are imported foaming furnace, it is foamed in foaming furnace; Mold temperature is controlled between 190 ℃; Foamed time is 1min, introduces the ventilation retrieving arrangement simultaneously, makes the hot gas flow of generation and the softening agent that volatilizes further cool off recycling; Guarantee that barometric point and ambient pressure in the stove remain basically stable; After the polyvinyl chloride resin product leaves foaming furnace air cooling 3s, roll stamp again and handle then, batch and obtain little foaming PVC matrix material.
Shown in accompanying drawing 3, little foaming PVC matrix material abscess evenly and not subsides, and abscess-size is 100-120 μ m, and density is 0.65g/cm
3
Little foaming PVC performance of composites is following:
Warp tensile strength 8.3MPa has improved 18.2% than existing technology, and weft tensile strength 7.5MPa has improved 8.9% than prior art, peel load 33N.
Claims (10)
1.PVC the composite modification whipping agent is characterized in that being made up of the raw material of following weight part:
1～5 part of whipping agent Cellmic C 121,2～5 parts of dispersion agents, foam stabilizer 0.5-2 part, Zinic stearas and zinc oxide proportioning are 0.5～1 part of compound, 0.1～2 part in the oxidation inhibitor of 2-5:1;
Above-mentioned raw materials is added in the mixing machine by said weight part, under 60～80 ℃ of conditions, mix 15～20min.
2. PVC composite modification whipping agent as claimed in claim 1 is characterized in that: said dispersion agent is to be to be formed according to the ratio of 1:1～5 is composite by whiteruss and Tristearoylglycerol.
3. PVC composite modification whipping agent as claimed in claim 1 is characterized in that: foam stabilizer is YSR 3286-polyoxy alkylene segmented copolymer, gather one or both mixtures in the methyl silicon SULPHOSUCCINIC ACID ESTER.
4. PVC composite modification whipping agent as claimed in claim 1; It is characterized in that: oxidation inhibitor is four [β-(3; The 5-di-tert-butyl-hydroxy phenyl) propionic acid] one or more mixtures in pentaerythritol ester, three ［ 2.4-di-tert-butyl-phenyl ］ phosphorous acid ester, β-positive octadecanol ester of (3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid.
5. PVC composite modification whipping agent as claimed in claim 1 is characterized in that: said modified foaming agent gas forming amount is 210-215ml/g, at 0-185 ℃ of Heat stability is good, rate of decomposition＜1%.
6. little foaming PVC matrix material; It is characterized in that raw material by following weight part; Through mixing, fusion plastification, foaming: 40～80 parts of SE (polymerization degree is 1000-2000), 1～5 part of the described modified foaming agent of claim 1 to 5,20～60 parts of superfine active calcium carbonates; 10～40 parts in softening agent, 0.5～5 part of thermo-stabilizer.
7. want 6 described little foaming PVC matrix materials like right, it is characterized in that: said superfine active calcium carbonate is the 1250-2500 order.
8. want 6 described little foaming PVC matrix materials like right, it is characterized in that: softening agent is one or both mixtures in Witcizer 300, the tributyl citrate.
9. want 6 described little foaming PVC matrix materials like right, it is characterized in that: said thermo-stabilizer is one or more mixtures in barium zinc composite stabilizer, thiol methyl tin, the antimony organic thermo-stabilizer.
10. the method for preparing the described little foaming PVC matrix material of claim 6-9 is characterized in that may further comprise the steps:
(1) mixing of materials: by the described proportioning of claim, with SE, modified foaming agent, superfine active calcium carbonate, softening agent, thermo-stabilizer add in the mixing machine, are under the 70-90 ℃ of condition in the material temperature, mix 15-25min;
(2) fusion plastification: the material of step (1) gained is plastified in Banbury mixer, and plasticization temperature is 130-150 ℃, and fusion time is 3-5min; Material with gained is transferred to further fusion plastification in two roller open mills then; Plasticization temperature is 140-160 ℃, and fusion time is 5-10min, will plastify then good material through travelling belt move in the four roller plastic calenders fit with base cloth after; The first and second roller temperature controls are at 165-175 ℃; The third and fourth roller temperature control is between 110-130 ℃, and roller speed is 30-45Hz/min, and traction is batched and obtained work in-process then;
(3) foaming: step (2) gained work in-process through the cylinder traction, are imported foaming furnace, and the mold temperature in the foaming furnace is between 180-210 ℃; Foamed time is 1-2min; After polyvinyl chloride resin leaves foaming furnace air cooling 3-5s, roll stamp again and handle, batch the acquisition finished product.
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| CN103161079A (en) * | 2013-03-29 | 2013-06-19 | 田学峰 | Manufacturing process of polyvinyl chloride artificial leather |
| CN103435935A (en) * | 2013-08-23 | 2013-12-11 | 吴江市英力达塑料包装有限公司 | Polyvinyl chloride soft foam plastic and preparation method thereof |
| CN103483718A (en) * | 2013-08-22 | 2014-01-01 | 中国科学院化学研究所 | Breathable artificial PVC (Polyvinyl Chloride) leather having micropore structure and preparation method thereof |
| CN104119652A (en) * | 2014-08-14 | 2014-10-29 | 苏州卓越工程塑料有限公司 | Flame-retardant PET |
| CN104927252A (en) * | 2015-07-14 | 2015-09-23 | 山东万图高分子材料有限公司 | Soft PVC foam materials containing plant extracts and preparation method thereof |
| CN111154147A (en) * | 2020-01-15 | 2020-05-15 | 张绍为 | Environment-friendly degradable buffer packaging material and preparation method thereof |
| CN111690217A (en) * | 2020-07-09 | 2020-09-22 | 浙江东部塑胶股份有限公司 | Micro-foaming polyvinyl chloride film and preparation method thereof |
| CN112724453A (en) * | 2020-12-23 | 2021-04-30 | 快思瑞科技(上海)有限公司 | Master batch material, preparation method of foaming master batch and preparation method of engineering plastic |
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| CN116041771A (en) * | 2023-02-09 | 2023-05-02 | 福州市福塑科学技术研究所有限公司 | Preparation method of flame-retardant anti-aging micro-foaming PVC composite material |
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| CN103161079A (en) * | 2013-03-29 | 2013-06-19 | 田学峰 | Manufacturing process of polyvinyl chloride artificial leather |
| CN103483718A (en) * | 2013-08-22 | 2014-01-01 | 中国科学院化学研究所 | Breathable artificial PVC (Polyvinyl Chloride) leather having micropore structure and preparation method thereof |
| CN103483718B (en) * | 2013-08-22 | 2016-01-06 | 中国科学院化学研究所 | Ventilative artificial PVC leather with microvoid structure and preparation method thereof |
| CN103435935A (en) * | 2013-08-23 | 2013-12-11 | 吴江市英力达塑料包装有限公司 | Polyvinyl chloride soft foam plastic and preparation method thereof |
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| CN111690217A (en) * | 2020-07-09 | 2020-09-22 | 浙江东部塑胶股份有限公司 | Micro-foaming polyvinyl chloride film and preparation method thereof |
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| CN116041771A (en) * | 2023-02-09 | 2023-05-02 | 福州市福塑科学技术研究所有限公司 | Preparation method of flame-retardant anti-aging micro-foaming PVC composite material |
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