CN103087442A - Method using Fe<3+> as PVC (Polyvinyl Chloride) assistant - Google Patents
Method using Fe<3+> as PVC (Polyvinyl Chloride) assistant Download PDFInfo
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- CN103087442A CN103087442A CN2012103032274A CN201210303227A CN103087442A CN 103087442 A CN103087442 A CN 103087442A CN 2012103032274 A CN2012103032274 A CN 2012103032274A CN 201210303227 A CN201210303227 A CN 201210303227A CN 103087442 A CN103087442 A CN 103087442A
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Abstract
The invention provides a method using Fe<3+> as a PVC (Polyvinyl Chloride) assistant. According to the invention, the influence of the content of Fe<3+> in a polymerization system on performance of polyvinyl chloride and optical performance of a polyvinyl chloride hard transparent sheet is researched through a lab-scale polymerization test of polyvinyl chloride.
Description
Technical field
The present invention is specifically related to a kind of Fe of utilization
3+Method as the PVC auxiliary agent.
Background technology
Polyvinyl chloride has mechanical property, anti chemical properties, erosion resistance and flame retardancy preferably, is widely used in to produce building pipe, sheet material and film, leatheroid, electric wire etc., and be large general-purpose plastics that energy consumption is low, cost is low, purposes is wide.In recent years, China's PVC Industry development is swift and violent, newly-built, expansion project starts one after another, production capacity enlarges rapidly, output significantly improves, but there is larger difference in the polyvinyl chloride quality that each enterprise produces, especially higher to performance requriements transparent article, and the polyvinyl chloride that some enterprise produces can not meet the demands.
According to the pertinent data introduction as can be known, the Fe that contains in raw material and various auxiliary agent (as vinyl chloride monomer, initiator, dispersion agent etc.)
3+Can produce adverse influence to polyreaction: 1. extend inductive phase, slowed down reaction speed; 2. make the thermal stability of polyvinyl chloride variation, the product tape look; 3. Fe
2+Can react with peroxide initiator, consume the part initiator, extend polymerization time.Therefore, in actual production and test, should strictly control Fe
3+Content.In order to investigate Fe
3+On the impact of polyvinyl chloride performance, destructive test has been carried out in invention, adds a certain amount of iron(ic) chloride in the polyvinyl chloride polymerization reaction system, the fundamental property of polyvinyl chloride and the optical property of polyvinyl chloride hard clear sheet after the investigation polymerization.
Summary of the invention
The invention provides a kind of Fe of utilization
3+As the method for PVC auxiliary agent, the present invention has studied Fe in polymerization system by the lab scale aggregation test of polyvinyl chloride
3+The impact of content on polyvinyl chloride performance and polyvinyl chloride hard clear sheet optical property.
1. one kind is utilized Fe
3+As the method for PVC auxiliary agent, it is characterized in that the preparation technology of sample is: according to the various materials of the accurate weighing of formula, it is added in mixing machine, high-speed mixing is put into low speed mixer to 105 ℃ of material temperatures, and to 40～50 ℃ of material temperatures, blowing is stand-by.Material plasticizing: material is compressing tablet on Brabender plasticizing instrument, and the material that plasticizing is good is put into rapidly press, is pressed into required sheet material, pressurize, is cooled to room temperature, takes out sample, and the square piece that is cut into 50 mm * 50 mm is to be tested.
2. the basic recipe of the described PVC of step 1: polyvinyl chloride resin, 100.0; Organotin TM-181,1.0～2.0; DOP, 0～10.0; AC-316A, 0～1.0; Pigment, appropriate.
3. the described polymerization technique of step 1: the monitoring device resistance to air loss, the spraying still release agent vacuumizes, add deionized water, initiator, dispersion agent, add chain-transfer agent the 1st time, vacuumize and get rid of oxygen in still, add vinyl chloride monomer, stir about 10 min, be warmed up to required polymerization temperature and begin polymerization, add chain-transfer agent the 2nd time after 1.5 h, add terminator after reaching the regulation pressure drop, reclaim unreacted vinyl chloride monomer, blowing, centrifugal, drying.
4. the described lab scale aggregation test of step 3 is filled a prescription (g): vinyl chloride monomer, 2700.0; Deionized water, 3790.0; Initiator, 9.00～10.00; Dispersion agent 1,20.00～25.00; Dispersion agent 2,8.000～10.000; Add chain-transfer agent, 1.000～2.000 the 1st time; Add chain-transfer agent, 1.000～2.000 the 2nd time; Terminator, 3.000～5.000; FeCl
3, variable.
Beneficial effect of the present invention is: the described Fe that adds tested number of step 3
3+Little on polymerization reaction time and transformation efficiency impact.
Add Fe in the described vinylchlorid lab scale of step 3 polymerization system
3+Obviously affected the polyvinyl chloride performance, plasticizer absorption reduces, whiteness and ageing whiteness variation, and molecular mass slightly increases, and it is large that particle diameter becomes, and size-grade distribution broadens.
The described optical property impact on polyvinyl chloride hard clear sheet of step 3 is larger, the transmittance variation, and yellowness index significantly increases.
Embodiment
The following examples elaborate to the present invention, but to not restriction of the present invention.
Embodiment 1
The present embodiment explanation Fe
3+The impact of content on the lab scale polymerization process performance of polyvinyl chloride adds FeCl in vinylchlorid lab scale aggregation test
3Solution adds respectively m (Fe in the investigation polymerization system
3+): m (VCM) is the Fe of 0,3,6,9 mg/kg
3+Impact on polyreaction bath temperature, polymerization temperature, polymerization pressure drop, polymerization time, transformation efficiency etc.The VCM suspension polymerization is thermopositive reaction, can grasp the changing conditions of material in reaction process, response intensity and reaction process by its exotherm, and the bath temperature curve can indirect reaction polymerization exotherm process.In the lab scale polymerization, reaction water bath temperature curve, polymerization temperature curve and polymeric kettle internal pressure curve are all more steady, and the Fe that adds tested number is described
3+Post-polymerization is steady.Fe
3+Content sees Table 1 to the impact of polymerization time and transformation efficiency.
As can be seen from Table 1, the Fe that adds tested number
3+Little on polymerization reaction time and transformation efficiency impact.
Table 1 Fe
3+The impact of content on polymerization time and transformation efficiency
| m(Fe 3+):m(VCM) /mg/kg | Polymerization time/min | Transformation efficiency/% |
| 0 | 310 | 85.9 |
| 3 | 312 | 87.6 |
| 6 | 322 | 86.9 |
| 9 | 316 | 86.3 |
Embodiment 2
The present embodiment explanation Fe
3+The impact of content on the polyvinyl chloride performance adds the Fe of tested number in the chloroethylene polymerization system
3+Little on the polymerization process impact, but larger on the impact of vinylchlorid lab scale polymerization product partial properties, see Table 2.
As known from Table 2, the resin outward appearance has obvious variation, adds m (Fe in polymerization system
3+): being a bit darkish in color of resin when m (VCM) is 6 mg/kg, as m (Fe
3+): when m (VCM) was 9 mg/kg, the color of resin was little yellow; The Fe that adds tested number
3+On the not impact of the apparent density of polyvinyl chloride (PVC) RESINS, but its plasticizer absorption, whiteness, ageing whiteness are with Fe
3+Increasing of add-on is downward trend; Number average molecular mass and weight average molecular mass are with Fe
3+Increasing gradually of add-on increases, as m (Fe
3+): when m (VCM) is 6 mg/kg, the molecular mass of resin has a higher value, and the molecular mass dispersion index does not change; Number average particle diameter, volume average particle size and size distribution index are with Fe
3+Increasing gradually of add-on increases.
Table 2Fe
3+Content is to the polyvinyl chloride (PVC) RESINS performance impact
Embodiment 3
The present embodiment explanation Fe
3+The impact of content on polyvinyl chloride hard clear sheet optical property, the factor that affects polyvinyl chloride hard clear sheet optical property is a lot, quality as polyvinyl chloride, various auxiliary agents, formulating of recipe and complete processing etc., wherein the quality of polyvinyl chloride plays critical effect, is determining transmittance, mist degree, yellowness index of goods etc.The general polyvinyl chloride that the selective polymerization degree is 700～800, ageing whiteness is high, thermal stability is good.The author has studied and has added tested number Fe in polymerization system
3+The optical property of polyvinyl chloride hard clear sheet, result is as shown in table 3.
From table 3 as can be known, along with Fe in polymerization system
3+The increase of content, the transmittance of polyvinyl chloride hard clear sheet descends gradually, and haze change is little, but the amplitude that yellowness index increases is very large.
Table 3 Fe
3+The impact of content on polyvinyl chloride hard clear sheet optical property
| m(Fe 3+)：m(VCM) / mg/ kg | Transmittance/% | Mist degree/% | Yellowness index |
| 0 | 89.2 | 5.2 | 5.3 |
| 3 | 88.3 | 5.9 | 7.5 |
| 6 | 87.6 | 5.3 | 10.4 |
| 9 | 86.4 | 5.5 | 14.5 |
Claims (4)
1. one kind is utilized Fe
3+Method as the PVC auxiliary agent is characterized in that:
According to the various materials of the accurate weighing of formula, it is added in mixing machine, high-speed mixing is put into low speed mixer to 105 ℃ of material temperatures, and to 40～50 ℃ of material temperatures, blowing is stand-by;
Material plasticizing: material is compressing tablet on Brabender plasticizing instrument, and the material that plasticizing is good is put into rapidly press, is pressed into required sheet material, pressurize, is cooled to room temperature, takes out sample, and the square piece that is cut into 50 mm * 50 mm is to be tested.
2. method according to claim 1 is characterized in that the basic recipe of PVC: polyvinyl chloride resin, 100.0; Organotin TM-181,1.0～2.0; DOP, 0～10.0; AC-316A, 0～1.0; Pigment, appropriate.
3. method according to claim 1, is characterized in that polymerization technique: monitoring device resistance to air loss, spraying still release agent, vacuumize, add deionized water, initiator, dispersion agent, add chain-transfer agent the 1st time, vacuumize and get rid of oxygen in still, add vinyl chloride monomer, stir about 10 min, be warmed up to required polymerization temperature and begin polymerization, 1.5 add chain-transfer agent the 2nd time after h, add terminator after reaching the regulation pressure drop, reclaim unreacted vinyl chloride monomer, blowing, centrifugal, drying.
4. method according to claim 3, is characterized in that lab scale aggregation test formula: vinyl chloride monomer, 2700.0 g; Deionized water, 3790.0 g; Initiator, 9.00～10.00 g; Dispersion agent 1,20.00～25.00 g; Dispersion agent 2,8.000～10.000 g; Add chain-transfer agent, 1.000～2.000 g the 1st time; Add chain-transfer agent, 1.000～2.000 g the 2nd time; Terminator, 3.000～5.000 g; FeCl
3, variable.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012103032274A CN103087442A (en) | 2012-08-24 | 2012-08-24 | Method using Fe<3+> as PVC (Polyvinyl Chloride) assistant |
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|---|---|---|---|
| CN2012103032274A CN103087442A (en) | 2012-08-24 | 2012-08-24 | Method using Fe<3+> as PVC (Polyvinyl Chloride) assistant |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1064086A (en) * | 1991-02-11 | 1992-09-02 | 齐鲁石油化工公司研究院 | Special material for medical polyvinyl chloride and preparation method thereof |
| CN1323839A (en) * | 2000-05-12 | 2001-11-28 | 罗姆和哈斯公司 | Plastic additives, improved method, products and articles made therefrom |
| CN101386661A (en) * | 2008-09-16 | 2009-03-18 | 浙江巨化股份有限公司电化厂 | Method for preparing polychloroethylene with high polymerization degree |
-
2012
- 2012-08-24 CN CN2012103032274A patent/CN103087442A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1064086A (en) * | 1991-02-11 | 1992-09-02 | 齐鲁石油化工公司研究院 | Special material for medical polyvinyl chloride and preparation method thereof |
| CN1323839A (en) * | 2000-05-12 | 2001-11-28 | 罗姆和哈斯公司 | Plastic additives, improved method, products and articles made therefrom |
| CN101386661A (en) * | 2008-09-16 | 2009-03-18 | 浙江巨化股份有限公司电化厂 | Method for preparing polychloroethylene with high polymerization degree |
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Application publication date: 20130508 |