CN107189266B - A kind of NCC and common enhanced foaming PVC of ultra-fine fibre glass - Google Patents

A kind of NCC and common enhanced foaming PVC of ultra-fine fibre glass Download PDF

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CN107189266B
CN107189266B CN201710480139.4A CN201710480139A CN107189266B CN 107189266 B CN107189266 B CN 107189266B CN 201710480139 A CN201710480139 A CN 201710480139A CN 107189266 B CN107189266 B CN 107189266B
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pvc
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fine fibre
fibre glass
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CN107189266A (en
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陈照峰
张俊雄
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Nanjing University of Aeronautics and Astronautics
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Nanjing University of Aeronautics and Astronautics
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    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
    • C08J9/08—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing carbon dioxide
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    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
    • C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
    • C08J9/102—Azo-compounds
    • C08J9/103—Azodicarbonamide
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
    • C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
    • C08J9/141—Hydrocarbons
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2203/00—Foams characterized by the expanding agent
    • C08J2203/02—CO2-releasing, e.g. NaHCO3 and citric acid
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2203/00—Foams characterized by the expanding agent
    • C08J2203/04—N2 releasing, ex azodicarbonamide or nitroso compound
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2203/00—Foams characterized by the expanding agent
    • C08J2203/14—Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2327/00—Characterised by the use 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; Derivatives of such polymers
    • C08J2327/02—Characterised by the use 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; Derivatives of such polymers not modified by chemical after-treatment
    • C08J2327/04—Characterised by the use 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; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
    • C08J2327/06—Homopolymers or copolymers of vinyl chloride
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    • C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
    • C08J2401/02—Cellulose; Modified cellulose
    • C08J2401/04—Oxycellulose; Hydrocellulose
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    • 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
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2237—Oxides; Hydroxides of metals of titanium
    • C08K2003/2241—Titanium dioxide
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/003—Additives being defined by their diameter
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/14—Applications used for foams

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  • Materials Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
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  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
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Abstract

The present invention is a kind of NCC and common enhanced foaming PVC of ultra-fine fibre glass, and the NCC enhanced foaming PVC is made of the NCC of 5~20nm of crystallite diameter, ultra-fine fibre glass, PVC masterbatch and the chemical assistant that avarage fiber diameter is 0.1~4 μm.The ratio of the NCC is 0.2~5%, NCC crystallite length, 150~400nm.The ratio of the ultra-fine fibre glass is 0.5~6.5%.The addition of NCC and ultra-fine fibre glass so that the foaming PVC of same volume while improving intensity and modulus, mention high void volume rate, reduce foaming PVC compaction rate, reached the light-weighted purpose of efficient and light weight.Meanwhile the bond strength that the use of NCC can be improved the bubbling efficiency of PVC, reduce foaming agent consumption, improve fiber and PVC, the production energy consumption and pollution of foaming PVC is effectively reduced.

Description

A kind of NCC and common enhanced foaming PVC of ultra-fine fibre glass
Technical field
The present invention relates to a kind of foamed polyvinyl chloride (PVC) and preparation methods, more particularly, to a kind of NCC (nanofiber Cellulose crystal) enhancing foaming PVC and preparation method, belong to foam material field.
Background technique
As a kind of good foamed plastics, foaming PVC is widely used for every field.It is formed according to foaming PVC Performance, the purposes of different foaming PVCs are also different, there is the ordinary rigid foaming PVC for general household floor, also have high speed to arrange The enhanced foaming PVC of vehicle or passenger plane.Glass, carbon fiber, wood-fibred, granular powder etc. are normally used for enhanced foaming PVC, have The advantages that modulus is high, intensity is big, good impact resistance, but its enhanced foaming PVC compactness is high, quality is larger, is difficult to realize foam The lightweight of PVC.NCC is as a kind of natural macromolecular compound from wood materials, and crystallite diameter is in 2~5nm, list Root fibre strength is up to 57GPa, can be applied to substitute traditional glass, carbon fiber, wood-fibred, granular powder to manufacture lightweight increasing Strong foaming PVC.
Application No. is 201410165145.7 Chinese patents to provide a kind of environment-friendly type wood-fibred Reinforced PVC composite shuttering And preparation method, by being formed after the mixing of polyvinyl chloride virgin material, reclaimed materials, wood powder and various chemical assistants through mixing, hot pressing, cold pressing After composite shuttering is made.The patent solves the problems, such as that traditional PVC reclaimed materials needs to separate hydrolysis, and preparation process flow letter Single, template is reused often.But the patent uses wood powder as reinforcing agent, wood powder non-refractory, in preparation process easily Smoke, and water content is difficult to control in wood powder, prepared PVC is fallen off in the long-term use with wood powder aging occurs, and PVC is old Change problem of Cracking, reduces the service life of composite PVC template.
The Chinese patent of Publication No. CN102617948A provides a kind of Fiberglass-reinforcePVC PVC sectional material and its preparation side Method, by being formed after the mixing of PVC raw material, short glass fiber, nanometer calcium carbonate and various modifying agent through extruder and extrusion die The PVC profile of glass fiber reinforcement is obtained afterwards.The patent solves traditional PVC profile high production cost, ineffective asks Topic, at the same prepared PVC profile bending strength is high, assembling processing technology is simple, it is light-weight, the spies such as fusion weld can be carried out Point.But the patent uses short glass fiber precursor as reinforcing fiber, brittleness is big, and intensity is low, and easy fragmentation, fiber is often It falls down, reduces the service life of PVC profile.
Summary of the invention
The purpose of the present invention overcomes the shortcomings of the prior art, and provide a kind of NCC enhances jointly with ultra-fine fibre glass Foaming PVC, by the NCC of 5~20nm of crystallite diameter, the ultra-fine fibre glass and PVC masterbatch that avarage fiber diameter is 0.1~4 μm Composition.The addition of NCC and ultra-fine fibre glass, so that the PVC foam strength of materials and abscess rate of same volume dramatically increase, It promotes intensity simultaneously, reduces bulk density, reached the light-weighted purpose of foaming PVC.Simultaneously NCC use increase PVC with it is ultra-fine The contact area of glass fibre reduces surface energy, avoids and occur stress concentration at foaming PVC median surface, failure easy to crack The problem of destruction, meanwhile, the addition of ultra-fine fibre glass improves the modulus of foaming PVC, improves its impact resistance.
To achieve the purpose of the present invention the technical solution adopted is that: provide a kind of NCC and increase jointly with ultra-fine fibre glass Strong foaming PVC, it is characterised in that the NCC enhanced foaming PVC is by the NCC of 5~20nm of crystallite diameter, avarage fiber diameter 0.1~4 μm of ultra-fine fibre glass, PVC masterbatch and chemical assistant composition.
The additive amount of NCC is 0.05~2.50% (weight percent), NCC crystallite ruler in the NCC enhanced foaming PVC Very little is diameter 5-20nm, length 150-400nm.
The ratio of ultra-fine fibre glass is 0.5~6.5% in the NCC enhanced foaming PVC, and fibre diameter is 0.1~4 Micron.
The chemical assistant includes 0.5~3% stabilizer, 1~2.5% titanium dioxide, 0.05~1.5% silane table Face modifying agent, 1.5~10% foaming agent, 0.1~4% blowing promotor, 0.5~2% lubricant and 3~6% plasticizer.
The foaming agent is sodium bicarbonate, n-hexane, hexamethylene or azodicarbonamide.
The blowing promotor is lead sulfate tribasic, dibasic lead phosphite, calcium stearate or zinc stearate.
The PVC masterbatch is the composition surplus of enhanced foaming PVC formula.
Preparation method includes the following steps:
1) ultra-fine fibre glass, NCC and titanium dioxide are carried out being sufficiently impregnated pre-processing respectively using silane surface modified dose, Wherein the ratio of silane surface modified dose and ultra-fine fibre glass is 1: 30~50, and silane surface modified dose and NCC of ratio is 1 : 10~20, the ratio of silane surface modified dose and titanium dioxide is 1: 3~8；
2) blowing promotor and foaming agent are uniformly mixed according to 1: 1.5~2.8 ratio；
3) after mixing PVC masterbatch, stabilizer and plasticizer under mixing machine 300~500rpm revolving speed, mixing machine is turned Speed is improved to 800~1000rpm and being heated to 80~110 DEG C melts addition material softening；
4) it keeps being added to pre-preg titanium dioxide, lubricant and pretreatment NCC under 800~1000rpm of mixing pan revolving speed In melt-mixed material, and revolving speed is improved to 1000~1200rpm；
5) mixing machine heating temperature is promoted to 115~135 DEG C, pre- place is added after being increased to 1500~1800rpm in revolving speed The ultra-fine fibre glass of reason is uniformly mixed addition material；
6) keep mixing disk rotating speed and reduce mixing machine temperature to after 90~110 DEG C, foaming agent is added and be sufficiently stirred 2~ After 3min, mixed material is discharged in low speed mixer to discharge after being cooled to 30~60 DEG C and obtains mixture；
7) heating and melting extrusion mixing material idiosome in extruder is added mixture into, it is cooling after 120~160 DEG C of foaming It is cut into NCC enhanced foaming PVC product.
Specific embodiment
Combined with specific embodiments below, the present invention is furture elucidated, it should be understood that these embodiments are merely to illustrate the present invention Rather than limit the scope of the invention, after the present invention has been read, those skilled in the art are to various equivalences of the invention It is as defined in the appended claims that the modification of form falls within the application.
Embodiment 1
A kind of NCC and common enhanced foaming PVC of ultra-fine fibre glass, it is characterised in that the NCC crystallite diameter is 3nm, 4 μm of ultra-fine fibre glass average diameter.
The ratio of the NCC is 2%, NCC crystallite length 200nm.
The ratio of the ultra-fine fibre glass is 1%.
The chemical assistant includes 1.5% stabilizer, 2% titanium dioxide, and silane surface modified dose of 0.05%, 3% Azodicarbonamide foaming agent, 1% calcium stearate blowing promotor, 1.5% lubricant and 3% plasticizer, surplus is PVC female Material.
The NCC enhanced foaming PVC's the preparation method comprises the following steps:
1) ultra-fine fibre glass, NCC and titanium dioxide are carried out being sufficiently impregnated pre-processing using silane surface modified dose, silane The ratio of surface modifier and ultra-fine fibre glass is 1: 30, and silane surface modified dose and NCC of ratio is 1: 10, silane surfaces The ratio of modifying agent and titanium dioxide is 1: 3；
2) blowing promotor and foaming agent are uniformly mixed according to 1: 1.6 ratio；
3) after mixing PVC masterbatch, stabilizer and plasticizer under mixing machine 500rpm revolving speed, mixing machine revolving speed is improved To 800rpm and being heated to 90 DEG C melts addition material softening；
4) it keeps being added to melt by pre-preg titanium dioxide, lubricant and pretreatment NCC under mixing pan 800rpm revolving speed mixing It closes in material, and improves revolving speed to 1000rpm；
5) mixing machine heating temperature is promoted to 120 DEG C, pretreated superfine glass is added after being increased to 1500rpm in revolving speed Fiber is uniformly mixed addition material；
6) it keeps mixing disk rotating speed and reduces mixing machine temperature to after after 90 DEG C, being added foaming agent and 2min is sufficiently stirred, Mixed material is discharged in low speed mixer to discharge after being cooled to 50 DEG C and obtains mixture；
7) heating and melting extrusion mixing material idiosome in extruder is added mixture into, the cooling cutting after 140 DEG C of foaming NCC enhanced foaming PVC product is made.
Embodiment 2
A kind of NCC and common enhanced foaming PVC of ultra-fine fibre glass, it is characterised in that the NCC crystallite diameter is 10nm, 2 μm of ultra-fine fibre glass average diameter.
The ratio of the NCC is that 3%, NCC crystallite length is 300nm.
The ratio of the ultra-fine fibre glass is 1.5%.
The chemical assistant includes 1.5% stabilizer, 1.2% titanium dioxide, and silane surface modified dose of 1%, 2% N-hexane foaming agent, 1% calcium stearate blowing promotor, 1.5% lubricant and 4% plasticizer, surplus are PVC masterbatch.
The NCC enhanced foaming PVC's the preparation method comprises the following steps:
1) ultra-fine fibre glass, NCC and titanium dioxide are carried out being sufficiently impregnated pre-processing using silane surface modified dose, silane The ratio of surface modifier and ultra-fine fibre glass is 1: 30, and silane surface modified dose and NCC of ratio is 1: 15, silane surfaces The ratio of modifying agent and titanium dioxide is 1: 8；
2) blowing promotor calcium stearate and foaming agent sodium bicarbonate are uniformly mixed according to 1: 2 ratio；
3) after mixing PVC masterbatch, stabilizer and plasticizer under mixing machine 500rpm revolving speed, mixing machine revolving speed is improved To 900rpm and being heated to 100 DEG C melts addition material softening；
4) it keeps being added to melt by pre-preg titanium dioxide, lubricant and pretreatment NCC under mixing pan 900rpm revolving speed mixing It closes in material, and improves revolving speed to 1200rpm；
5) mixing machine heating temperature is promoted to 120 DEG C, pretreated superfine glass is added after being increased to 1400rpm in revolving speed Fiber is uniformly mixed addition material；
6) it keeps mixing disk rotating speed and reduces mixing machine temperature to after after 100 DEG C, being added foaming agent and 3min is sufficiently stirred, Mixed material is discharged in low speed mixer to discharge after being cooled to 50 DEG C and obtains mixture；
7) heating and melting extrusion mixing material idiosome in extruder is added mixture into, the cooling cutting after 110 DEG C of foaming NCC enhanced foaming PVC product is made.
It above are only the single specific embodiment of the present invention, but the design concept of the present invention is not limited to this, all utilizations This design makes a non-material change to the present invention, and should belong to the behavior for invading the scope of protection of the invention.But it is all not It is detached from the content of technical solution of the present invention, it is to the above embodiments any type of simple according to the technical essence of the invention Modification, equivalent variations and remodeling, still fall within the protection scope of technical solution of the present invention.

Claims (2)

1. a kind of NCC and common enhanced foaming PVC of ultra-fine fibre glass, ingredient are as follows:
0.2~5% NCC, diameter 5-20nm, length 150-400nm；
0.5~6.5% ultra-fine fibre glass, 0.1~4 μm of diameter；
1~2.5% titanium dioxide；
Chemical assistant includes:
0.5~3% stabilizer,
Silane surface modified dose of 0.05~1.5%,
1.5~10% foaming agent,
0.1~4% blowing promotor,
0.5~2% lubricant
3~6% plasticizer；
The foaming agent is sodium bicarbonate, n-hexane, hexamethylene or azodicarbonamide；
The blowing promotor is lead sulfate tribasic, dibasic lead phosphite, calcium stearate or zinc stearate；
The PVC masterbatch is the composition surplus of enhanced foaming PVC formula.
2. the foaming PVC preparation method that a kind of NCC and ultra-fine fibre glass enhance jointly, it is characterised in that the preparation method packet Include following steps:
1) ultra-fine fibre glass, NCC and titanium dioxide are carried out being sufficiently impregnated pre-processing respectively using silane surface modified dose, wherein The ratio of silane surface modified dose and ultra-fine fibre glass is 1: 30~50, and silane surface modified dose and NCC of ratio is 1: 10 ~20, the ratio of silane surface modified dose and titanium dioxide is 1: 3~8；
2) blowing promotor and foaming agent are uniformly mixed according to 1: 1.5~2.8 ratio；
3) after mixing PVC masterbatch, stabilizer and plasticizer under mixing machine 300~500rpm revolving speed, mixing machine revolving speed is mentioned Up to 800~1000rpm and be heated to 80~110 DEG C make be added material softening melting；
4) it keeps that pre-preg titanium dioxide, lubricant and pretreatment NCC are added to melting under 800~1000rpm of mixing pan revolving speed In mixture, and revolving speed is improved to 1000~1200rpm；
5) mixing machine heating temperature is promoted to 115~135 DEG C, revolving speed be increased to after 1500~1800rpm be added it is pretreated Ultra-fine fibre glass is uniformly mixed addition material；
6) it keeps mixing disk rotating speed and reduces mixing machine temperature 2~3min simultaneously is sufficiently stirred to foaming agent after 90~110 DEG C, is added Afterwards, mixed material is discharged in low speed mixer to discharge after being cooled to 30~60 DEG C and obtains mixture；
7) heating and melting extrusion mixing material idiosome in extruder is added mixture into, cools down, cut after 120~160 DEG C of foaming It cuts and NCC enhanced foaming PVC product is made.
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CN109810434A (en) * 2019-03-04 2019-05-28 嘉兴市南湖高分子材料有限公司 Expansion type polyvinyl chloride packing material and preparation method thereof
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