CN1137201C - Process for preparation polyvinyl-chloride foaming material - Google Patents
Process for preparation polyvinyl-chloride foaming material Download PDFInfo
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- CN1137201C CN1137201C CNB991238133A CN99123813A CN1137201C CN 1137201 C CN1137201 C CN 1137201C CN B991238133 A CNB991238133 A CN B991238133A CN 99123813 A CN99123813 A CN 99123813A CN 1137201 C CN1137201 C CN 1137201C
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Abstract
The present invention discloses a production method for PVC foam with a high foaming ratio, which comprises the steps that after being measured according to the formula, scorched PVC resin, plasticizers, foaming agents, processing aiding agents, etc. are stirred and evenly mixed, and after the processes of gelatinization, plasticization and foaming are carried out, the materials are cooled and cut so as to manufactured into the PVC foam plastic with a high foaming ratio as a finished product.
Description
The present invention relates to a kind of preparation method of high foamability foam material.More particularly, the present invention relates to the preparation method of polyvinyl chloride (PVC) high foamability foam material.
As everyone knows, porous plastics be a kind of be the matrix material of filler with gas, compare with plastics, it has many valuable performances, as light weight, specific tenacity height, to absorb the strong and heat-insulating sound-insulating of shock load ability effective etc.Therefore, be extensive use of in the industries such as automobile, electronics, chemical industry and machinery.
Because the method that the molecular structure of various resins adopts during with microscopic pattern and foaming is different, thus cause melt tension different with elasticity, thereby directly influence the multiplying power when plastic foamed.Some material for example polyethylene (PE), urethane (PU) more easily foams, and expansion ratio can reach about 20 times.When the chemical process of some material as PVC adopts foamed, expansion ratio can only reach 3-4 doubly, and it is just very difficult to increase multiplying power again.
In order to improve the expansion ratio of plastic material, two kinds of methods are arranged roughly: a kind of method is the resin of exploitation high fondant-strength, as the PP-FAS-814 of U.S. Himont company; Another kind method is to improve existing foaming method.
Company of Total France adopts freonll-11 and chemical foaming to combine, and obtains the PVC foam material of 20-27 times of expansion ratio with two steps or three-step approach foaming.
There are the dielectric expansion of employing method in Korea S and the Mitsubishi company of changing into, preparation high foamability PVC material.Also having the part Study personnel to adopt blending resin to make expansion ratio is PVC material about 6 times.
We are through research chronically, and chemical foaming agent is adopted in test repeatedly, and making unit weight by a step foaming and two step foamings (another part application) is 90-240kg/m
3, expansion ratio is the PVC foam material more than 20 times.
Therefore, order of the present invention provides the manufacture method of the PVC foam material of high foamability.
More particularly, method provided by the invention is to stick with paste resin to be coated with the method for scraping.It is PVC to be stuck with paste resin, softening agent, whipping agent, foam stabilizer, processing aid, filler and pigment mix that described paste resin is coated with the method for scraping, after making slurry, be coated on the paper tape, obtain the different PVC foam material product of expansion ratio through gel, plasticizing, melt foaming, cooling and cutting.
Prescription raw materials used in the inventive method is:
Formulation weight part
PVC sticks with paste resin 100
Softening agent 35-120
Whipping agent 5-20
Linking agent 0.1-5
Foam stabilizer 0-10
Thermo-stabilizer 0.5-10
Filler 0.5-50
Lubricant is an amount of
Pigment is an amount of.
Used raw material PVC sticks with paste resin and is selected from emulsion seeding polymerization method PVC and sticks with paste resin, emulsion continuous polymerization PVC and stick with paste resin, emulsion and do not have seeding polymerization method PVC and stick with paste that resin, emulsion swollen-state polymerization method PVC are stuck with paste resin, microsuspension method PVC sticks with paste at least a or its several paste resins in resin, seed microsuspension method polyvinyl chloride resin or the breast-little hybrid system polyvinyl chloride resin in the inventive method.Their denominator is that the granularity of the primary particle of paste resin is 0.2-2.0 μ.Dried resin size 30-70 μ.In softening agent, can " disintegration " be primary particle, to make stable plastipaste material.
When preparing plastipaste in the methods of the invention, employed softening agent is crucial.Softening agent is a PVC plastipaste chief component, and in plastipaste, a softening agent part is as sticking with paste the moistening certain thickness immovable bed of resin surface; Another part is filled in as medium and sticks with paste between the resin particle gap; Rest part is as intergranular free-pouring softening agent.Therefore softening agent is the dispersion medium of suspension system, influences foam structure, snappiness, low-temperature performance, flame retardant resistance, smell and migration performance etc. that PVC sticks with paste resin flow performance, product.Employed softening agent is selected from by n-butyl phthalate (DBP) in the inventive method, dinoctyl phthalate (DOP), didecyl phthalate (DDP), Phthalic acid, diallyl ester (DAP), diethyl phthalate (DEP), diheptyl phthalate (DHP), diphenyl phthalate (DPP), dimethyl phthalate, diisobutyl phthalate (DMP), dimixo-octyl phthalate (DIOP), at least a or its combination in diisooctyl isophthalate (DIOIP) or the dioctyl isophthalate composition group.It is 100 weight parts that its consumption is stuck with paste resin by PVC, and softening agent is the 35-120 weight part, is preferably the 40-100 weight part, more preferably the 50-90 weight part.When plasticizer consumption was less than 35 weight parts, expansion ratio was low, and when plasticizer dosage surpassed 120 weight parts, expansion ratio began to reduce, and this may be because the viscosity of system is excessive or too smallly all be unfavorable for high foaming.Certainly, the temperature of system is also very important to high foamability.
Employed in the methods of the invention whipping agent is that gas forming amount is big, the high organic blowing agent of foaming efficient.For the plastipaste system, product requirement reaches high foamability, selects efficient aerating powder also very important.Whipping agent of the prior art can be divided into: (1) azo compound; (2) N-nitroso compound; (3) hydrazide kind compound; (4) urea derivative; (5) triazo-compound etc.In the inventive method employed whipping agent be selected from the inferior methyne tetramine of Cellmic C 121 (AC), dinitroso, to sulfonyloxy methyl amine, Diisopropyl azodicarboxylate (AZDN), 4, at least a or several in 4 '-bis oxide benzol sulfohydrazide or the sodium bicarbonate composition group.Its consumption is pressed PVC and is stuck with paste resin 100 weight, and whipping agent is the 5-20 weight part, is preferably the 7-18 weight part, more preferably the 9-14 weight part.Be lower than 5 weight parts, the expansion ratio that misses one's aim is higher than 20 weight parts, and expansion ratio and abscess quality can descend on the contrary.This is because whipping agent can exothermic cause in decomposition course.Whipping agent is many more, and it is big more to foam, and the heat of generation is just many more.When abscess formation in a single day, abscess has just become hot poor conductor, and it makes melt viscosity and melt tension descend, and at this moment also steeping to break to steep greatly increases, so expansion ratio descends on the contrary.
Employed linking agent is selected from by dicumyl peroxide (DCP) or benzoyl peroxide among the present invention, and its consumption is stuck with paste resin 100 weight parts for pressing PVC, and linking agent is the 0.1-5 weight part, is preferably the 0.5-4 weight part, more preferably the 1-3 weight part.
In order to make uniform in foaming, use foam stabilizer in the methods of the invention, also can not use foam stabilizer, its consumption is pressed PVC and is stuck with paste resin 100 weight parts, foam stabilizer is the 0-10 weight part, be preferably the 1-9 weight part, 3-8 weight part more preferably, foam stabilizer are selected from by methyl-silicone oil, phenyl silicone oil, tolyl silicone oil or containing hydrogen silicone oil forms at least a or several in the group.
Owing to the defective of polyvinyl chloride molecular chain itself, cause the poor heat stability of polyvinyl chloride molecule.For foaming process is successfully carried out, added thermo-stabilizer in the inventive method, its consumption is pressed PVC and is stuck with paste resin 100 weight parts, and thermo-stabilizer is the 0.5-10 weight part, is preferably the 1-8 weight part, more preferably the 3-7 weight part.Employed stablizer is selected from by the base lead salt class in the inventive method, as dibasic lead stearate, second base lead sulfate or dibasic lead phosphite; The metallic soap class is as calcium stearate, barium stearate, cadmium stearate, Zinic stearas, lead stearate or cadmium laurate; Organic tin is as dibutyl tin laurate, toxilic acid dioctyltin, two lauric acid, two positive phenyltins, two (the different monooctyl ester of sulfo-glycolic acid) two positive phenyltins or two (the different monooctyl ester of sulfo-glycolic acid) di-n-butyl tin; One package stabilizer is as at least a or its combination in liquid organic calcium zinc complexes, the organic barium zinc complexes of liquid or the organic barium cadmium of the liquid mixture composition group.
Employed in the present invention processing aid also has lubricant, filler and pigment etc. except thermo-stabilizer.They all are well-known in the art.For example, use the moderate lubrication agent, lubricant is selected from stearic acid and ester class such as stearic acid; The metallic soap class is as hard acid calcium, barium stearate, cadmium stearate, Zinic stearas or lead stearate; Hydro carbons is as at least a or its combination in paraffin, polyethylene wax or the oxidic polyethylene composition group.Used filler in the inventive method, press PVC and stick with paste resin 100 weight parts, amount of filler is the 0.5-50 weight part, is preferably the 1-40 weight part, 10-35 weight part more preferably, filler can be selected from least a or several in talcum powder, silicon-dioxide, lime carbonate or the wollastonite composition group.
Method of the present invention can be used the PVC porous plastics of the device fabrication high foamability of suitable treatment plastics with very high efficient.Method of the present invention is to comprise that PVC sticks with paste the raw material of processing aid general in resin, softening agent, whipping agent and the technological process etc., after the prescription metering, adds in the steel basin.Following in room temperature stirs raw mix with 50-400 rev/min, makes it generate the mixing raw material material of pulpous state.
The pulpous state mixing raw material material of preparation is coated on the release paper tape with coating method, chart drive speed be 1-10 rice/minute, preferred 3-9 rice/minute, more preferably 5-8 rice/minute.Enter drying tunnel then, in drying tunnel, under 120 ℃ of-240 ℃ of temperature, after gelling, plasticizing and foaming, make the PVC porous plastics of high foamability, its performance is as follows:
Thickness 2-8mm
Appearance white, micropore, foam are even
Density 90～150kg/m
3
Can ratio-frequency welding, fire-retardant
Mechanical property:
Tensile strength 〉=0.2Mpa
Elongation at break 〉=100%
Compressive strength P50/1 〉=25KPa
The device of implementing the inventive method is a device general in the present technique field, as colloidal mill TN-50 type (Beijing space flight and aviation machine works), steel basin be coated with fabric belt (Kunshan, Shanghai machine works) etc.
Testing sequence is:
(1) step of preparation mixing raw material pasty material
In steel basin, after powdered auxiliary agent such as thermo-stabilizer and part softening agent one reinstated colloidal mill or three-roller and grind, add the remainder that PVC sticks with paste resin and softening agent by prescription again, stirring pulping homogenizing, the pasty material of the raw mix that preparation mixes;
(2) coating, gel and foaming step
With the pasty material of the mixing raw material of step (1) preparation, the release paper tape that thickness on request is coated on band material on the separate-type paper belt surface of transmission constantly enters the drying tunnel of 110 ℃-240 ℃ of temperature section controls, and pulp gel and foaming are carried out continuously;
(3) cooling, side cut and rolling step
Sheet material after the foaming is peeled off through cooling and with separate-type paper, is wound into product.
Further describe the present invention with embodiment below.These examples are preferred embodiment of the invention, are not construed as limiting the invention.
Test conditions as mentioned above.Those skilled in the art can select arbitrarily in above-mentioned scope, no longer repeat at this.The composition of raw materials of each embodiment is listed in the table below.
Zero expression is excellent; represents very.
| Embodiment | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 |
| PVC (weight part) | 100 | 100 | 100 | 100 | 100 | 100 | 100 | 100 |
| DOP (weight part) | 75 | 75 | 50 | - | 60 | 75 | 50 | 75 |
| DBP (weight part) | - | - | - | 80 | - | - | 10 | - |
| DAP (weight part) | - | - | 30 | - | - | - | 10 | - |
| DOIP (weight part) | - | - | - | - | 20 | - | - | - |
| AC (weight part) | 4 | - | 8 | 6 | 6 | 8 | 4 | 8 |
| AZDN (weight part) | - | 6 | - | - | - | - | 4 | - |
| Foam stabilizer (weight part) | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
| Compound barium zinc (weight part) | - | 4 | - | - | - | - | 5 | - |
| Lead salt (weight part) | 4 | - | 4 | - | - | 6 | - | - |
| Organotin (weight part) | - | - | - | 5 | 5 | - | - | 8 |
| Lime carbonate (weight part) | 10 | 10 | 10 | - | 8 | 10 | - | 10 |
| Silicon oxide (weight part) | - | - | - | 10 | 2 | - | 5 | - |
| The result | ||||||||
| Spumescence | ○ | ○ | □ | □ | ○ | □ | □ | ○ |
| Unit weight (Kg/m 3) | 150 | 107 | 96 | 110 | 108 | 96 | 129 | 95 |
After the description of reading above, those skilled in the art can make the present invention the present invention and improve or revise, only otherwise leave spirit of the present invention, and all in model of the present invention.Scope of the present invention is proposed by the appended claims.
Claims (10)
1. the preparation method of a polyvinyl-chloride foam material, this method comprises:
By following prescription
Formulation weight part
Pvc resin paste grade 100
Softening agent 35-120
Whipping agent 5-20
Linking agent 0.1-5
Foam stabilizer 0-10
Filler 0.5-50
Thermo-stabilizer 0.5-10
Pigment is an amount of
Lubricant is an amount of
Above-described pvc resin paste grade is selected from not to be had seeding polymerization method pvc resin paste grade, emulsion swollen-state polymerization method pvc resin paste grade, microsuspension method pvc resin paste grade, seed microsuspension method pvc resin paste grade or breast-little hybrid system pvc resin paste grade by emulsion seeding polymerization method pvc resin paste grade, emulsion continuous polymerization pvc resin paste grade, emulsion and forms at least a in the group or its several pastes trees. fat; Described linking agent is selected from dicumyl peroxide or benzoyl peroxide;
(1) with after the raw material metering, at room temperature, stirs described raw material, make its uniform mixing, make pulpous state mixing raw material material;
(2) the pulpous state mixing raw material material of (1) preparation, be coated on the release paper tape, heating continuously, temperature is 110 ℃-240 ℃, makes its gel and foaming;
(3) cooling back cutting.
2. by the preparation method of the described polyvinyl-chloride foam material of claim 1, wherein said prescription is:
Formulation weight part
Pvc resin paste grade 100
Softening agent 40-100
Whipping agent 7-18
Linking agent 0.5-4
Foam stabilizer 1-9
Filler 1-40
Thermo-stabilizer 1-8
Pigment is an amount of
Lubricant is an amount of.
3. by the preparation method of the described polyvinyl-chloride foam material of claim 1, wherein said prescription is:
Formulation weight part
Pvc resin paste grade 100
Softening agent 50-90
Whipping agent 9-14
Linking agent 1-3
Foam stabilizer 3-8
Filler 10-35
Thermo-stabilizer 3-7
Pigment is an amount of
Lubricant is an amount of.
4. by the preparation method of the described polyvinyl-chloride foam material of claim 1, wherein softening agent is selected from by n-butyl phthalate, dinoctyl phthalate, didecyl phthalate, Phthalic acid, diallyl ester, diethyl phthalate, diheptyl phthalate, diphenyl phthalate, dimethyl phthalate, diisobutyl phthalate, dimixo-octyl phthalate, diisooctyl isophthalate or dioctyl isophthalate and forms at least a or its combination in the group.
5. press the preparation method of the described polyvinyl-chloride foam material of claim 1, wherein said whipping agent is selected from by the inferior methyne tetramine of Cellmic C 121, dinitroso, to sulfonyloxy methyl amine, Diisopropyl azodicarboxylate, 4, at least a or several in 4 '-bis oxide benzol sulfohydrazide or the sodium bicarbonate composition group.
6. by the preparation method of the described polyvinyl-chloride foam material of claim 1, wherein said foam stabilizer is selected from by methyl-silicone oil, phenyl silicone oil, tolyl silicone oil or containing hydrogen silicone oil forms at least a or several in the group.
7. by the preparation method of the described polyvinyl-chloride foam material of claim 1, wherein said thermo-stabilizer is selected from by base lead salt class, metallic soap class, organic tin, one package stabilizer forms at least a or its combination in the group.
8. by the preparation method of the described polyvinyl-chloride foam material of claim 7, wherein said thermo-stabilizer is selected from by dibasic lead stearate, second base lead sulfate, dibasic lead phosphite, calcium stearate, barium stearate, cadmium stearate, Zinic stearas, lead stearate, cadmium laurate, dibutyl tin laurate, the toxilic acid dioctyltin, two lauric acid, two positive phenyltins, two (the different monooctyl ester of sulfo-glycolic acid) two positive phenyltins, two (the different monooctyl ester of sulfo-glycolic acid) di-n-butyl tin, liquid organic calcium zinc complexes, the organic barium zinc complexes of liquid, at least a or its combination in the organic barium cadmium of the liquid mixture composition group.
9. by the preparation method of the described polyvinyl-chloride foam material of claim 1, at least a or several in the optional free skating stone flour of wherein said filler, silicon-dioxide, lime carbonate or the wollastonite composition group.
10. by the preparation method of the described polyvinyl-chloride foam material of claim 1, when wherein mixing, the temperature of described raw mix material remains on 60 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB991238133A CN1137201C (en) | 1999-11-12 | 1999-11-12 | Process for preparation polyvinyl-chloride foaming material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB991238133A CN1137201C (en) | 1999-11-12 | 1999-11-12 | Process for preparation polyvinyl-chloride foaming material |
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| CN1296031A CN1296031A (en) | 2001-05-23 |
| CN1137201C true CN1137201C (en) | 2004-02-04 |
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| CNB991238133A Expired - Lifetime CN1137201C (en) | 1999-11-12 | 1999-11-12 | Process for preparation polyvinyl-chloride foaming material |
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1999
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