CN101033309A - Color masterbatch for polythene and preparing method thereof - Google Patents
Color masterbatch for polythene and preparing method thereof Download PDFInfo
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Abstract
The invention relates to a kind of color masterbatch of polyethylene and its preparation method. The color masterbatch includes following components: a. carrier resin, including polyethylene resin, EVA or the mixture of the two kinds of resin. b. carbon black. c. surface treatment agent of coupling group. d. dispersant. In which, it takes the weight of the carrier resin as 100 weight share, then it has 40 ~ 180 weight share of the described carbon black, 0.5 ~ 20 weight share of the surface treatment agent, 1~20 weight share of the dispersant. In the invention, it handles the carbon black by using the surface treatment agent, and then it mixes with the carrier resin through banburying, after that, it melts and extrudes it with the dispersant to achieve the material.
Description
Technical field
The present invention relates to a kind of color masterbatch for polythene, be specifically related to a kind of polyvinyl piping materials carbon black masterbatch and preparation method thereof.
Background technology
Polyethylene (PE) resin is one of main raw material(s) of plastic pipe, and characteristics such as, save energy in light weight, corrosion-resistant with it more and more come into one's own, and Application Areas is also increasing.At present, polyvinyl piping materials has partly substituted metal tube.In the annual growth of the PE of developed country pipe more than 2.5%, its consumption is only second to polyvinyl chloride, be second largest plastic conduit kind of consumption in the world, be widely used in fields such as engineerings such as feedwater, agricultural irrigation, combustion gas conveying, blowdown, mine mortar conveying and oil field, chemical industry, post and telecommunications.
In poly a lot of purposes (as film), polyethylene basis resin can no longer be equipped with any additives and use separately, or only is used for painted purpose and colour batch.In this case, has been furnished with the oxidation inhibitor that satisfies the process requirements amount in resin processing plant usually.But for the material of making polyvinyl piping materials, usually should comprise two stabilising systems, and must satisfy longer stabilising effect: one is oxidation-stabilized system, its effect be guarantee the PE resin in being processed into the process of tubing, the secondary of tubing is heated and unlikelyly in (as welding) and the use suffers oxidation destruction; One is the light stabilising system, and assurance tubing is avoided the destruction of uv-radiation at lay up period with between the usage period.For the ultra-violet resistance energy of PE tubing, common way is to add a certain amount of carbon black in the PE base-material.China is 2.5 ± 0.5wt% to the requirement of carbon black content in the polyethylene water service pipe material, and carbon black dispersion degree is answered≤3 grades (GB/T 13663-2000); It is 2～2.6wt% that carbon black content in the PE gas line material is required; Carbon black content is between 2～2.5wt% in the regulation PE gas line raw material among the ISO4437-1997, and carbon black diffusion grade is answered≤3 grades.
At present, polyvinyl piping materials manufacturer adopts the PE pellet usually, uses single screw extrusion machine extrusion moulding PE tubing.For polyethylene penstock material, in order to guarantee the dispersion effect of carbon black in tubing, Tong Hang method is directly to be produced by production of resins factory to comprise the necessary stabilising system tube material of (comprising the specified amount carbon black) in the world, domestic PE tube material manufacturer carries out modification by the base resin that resin processing plant is produced, add specified amount carbon black and dispersion agent, can increase the production cost of tube material so undoubtedly, and in the process of adding carbon black, cause the decline of PE resin mechanical property easily; The tubing way that another manufacturing cost is lower is the factory at tubing, base resin and carbon black masterbatch are carried out mechanically mixing earlier, then directly by extruder for shaping tubing, in this kind method, in order to improve the dispersity of carbon black, extrusion equipment had special requirement, when on the common PE tube extruding equipment, adopting this method to carry out extruding of tubing, because common carbon black look mother's is dispersed relatively poor, the dispersion effect of carbon black is relatively poor in institute's extruding pipe material, does not satisfy the requirement of relevant pipe standard.
Summary of the invention
At the problems of the prior art, the purpose of this invention is to provide a kind of polyethylene high concentration carbon black masterbatch, adopt this black masterbatch and PE tubing base-material to adopt conventional single screw rod pipe extruder to extrude, just can obtain the good polyvinyl piping materials of carbon black dispersion degree.
The present invention also provides the preparation method of polyethylene usefulness high concentration carbon black masterbatch in this, and technology is simple, and processing ease is suitable for industrial application.
A kind of color masterbatch for polythene of the present invention includes the following component of blend: a. vector resin, b. carbon black, c. surface treatment agent, d. dispersion agent.Be 100 parts in the vector resin parts by weight wherein, described carbon black is 40～180 parts, is preferably 80～150 parts; Described surface treatment agent is 0.5～20 part, is preferably 1～10 part; Described dispersion agent is 1～20 part, is preferably 5～15 parts.
The vector resin of the above component a comprises the disclosed various types of polyvinyl resins of prior art, ethylene-vinyl acetate copolymer (EVA) resin etc., perhaps is the mixture of the above resin.The consistency of these two kinds of vector resins of the present invention and PE tube material is good, and carbon black easily disperses in these two kinds of resins, thereby can make that the carbon black dispersion effect is good in the polyvinyl piping materials of final preparation.From with the consistency and the carbon black dispersion therein of polyethylene pipe material, EVA or itself and poly mixture effect are better, vector resin of the present invention is preferably ldpe resin (LDPE), EVA or its mixing.But consider the cost problem, more preferably new LDPE (film grade).
The carbon black of the above components b can comprise disclosed all kinds carbon black in the prior art, the uvioresistant effect of material is better when proving black grain diameter≤30nm after deliberation, but when particle diameter≤10nm, force of cohesion between the particle strengthens, the dispersing property variation that causes carbon black, be unfavorable for that carbon black is evenly dispersed, and influences the performance of uvioresistant performance in the PE tube material.Therefore the median size at carbon black described in the color masterbatch for polythene of the present invention is 10～30nm, is preferably 15～25nm.
The surface treatment agent of the above amount of component b is the auxiliary agent that is used for the mineral dye surface activation process, also is called coupling agent, comprises at least a in the following material: titanate coupling agent, aluminate coupling agent, silane coupling agent, soap or stearate; Wherein be preferably titanate coupling agent.
The dispersion agent of the above component d comprises at least a in the following material: oxidic polyethylene, polyethylene wax, stearic acid, stearate, solid paraffin, whiteruss, dioctyl phthalate (DOP) (DOP), turps, triphenylphosphate or ethylene bis stearamide etc. can make this system have the good distribution effect; Wherein preferably include at least a in the following material: polyethylene wax, stearic acid or ethylene bis stearamide.
In addition, color masterbatch for polythene of the present invention also can include the conventional auxiliary agent that polyethylene is used, as processing aids such as lubricant, oxidation inhibitor.Wherein lubricant such as calcium stearate, Zinic stearas etc.; Oxidation inhibitor is the conventional oxidation inhibitor of polyethylene, as antioxidant 1076,1010, and auxiliary antioxidant DLTP, DSTP etc.The consumption of usual auxiliaries is a conventional amount used, or adjusts according to practical requirements.
Color masterbatch for polythene of the present invention, it is prepared by the method that may further comprise the steps:
1. the above carbon black and surface treatment agent are pressed the even blend of described consumption;
2. will comprise the step 1. carbon black handled of surface treatment agent, component banburying in Banbury mixer of the above vector resin, mix, after the discharging, compressing tablet, pulverizing;
3. with step 2. after the pulverizing material of gained and the above dispersant melt blending obtain the good high concentration of polyethylene of described dispersing property and use the look mother.
Among the preparation method of color masterbatch for polythene of the present invention, the vector resin parts by weight are 100 parts of meters, and described carbon black is 40～180 parts, are preferably 80～150 parts; Described surface treatment agent is 0.5～20 part, is preferably 1～10 part; Described dispersion agent is 1～20 part, is preferably 5～15 parts.
Among the preparation method of above-described color masterbatch for polythene of the present invention, step can be mixed surface treatment agent and carbon black by mechanical blending general in the prior art and method in 1..The preferred homogenizer that uses mixes, stirring velocity 100～3000rpm, and the treatment time generally can be between 0.5～10min.General increase the treatment time and can improve and show treatment effect, but can influence working (machining) efficiency simultaneously.
Among the preparation method of above-described color masterbatch for polythene of the present invention, the surface-treated carbon black that 1. step obtains vector resin, step in 2. and other conventional auxiliary agents as oxidation inhibitor one class are put into Banbury mixer and are carried out banburying.The banburying process need not indirect heating, and vector resin can fusion under the situation that self friction heats up.General in this case banburying built-in temperature is 50～135 ℃, and better effects if is 80～130 ℃.In this step, carbon black granules is pulverized and be dispersed in carbon black in the vector resin uniformly by the powerful frictional force between resin and the carbon black; Banburying mixes the back discharging.Blended stock is placed in two roller mills while hot is pressed into sheet material, carry out pulverization process after the cooling.
Among the preparation method of above-described color masterbatch for polythene, the melt blending of step in 3. can adopt common melt-mixing equipment and technology in the prior art.Preferably utilize screw extrusion press (single screw extrusion machine or twin screw extruder) that described material is carried out melt blending, the melt blending temperature is 60～180 ℃.
The present invention proposes a kind of color masterbatch for polythene and preparation method thereof, adopt its carbon black content height of black masterbatch (can up to about 60%) of this method preparation, and have good dispersing property.After carrying out simple and mechanical blend with PE tubing base-material, adopting conventional single screw rod pipe extruder to carry out tubing extrudes, the carbon black dispersion degree of the tubing of being extruded is good, meet the countries concerned's standard-required (≤3 grades), greatly simplified the course of processing of PE tubing, and cut down finished cost effectively.And, extrude ratio (the look mother of the present invention: the polyethylene base-material) can reach 1: 20 (carbon black content 〉=2.0% of institute's extruding pipe material at this moment) who adds the consumption in man-hour at tubing owing to carbon black content height among the look mother.PE tubing of the present invention has a good application prospect with the processing of extruding that high heavy colour mother can be widely used in PE tubing.
Embodiment
Further describe the present invention below in conjunction with embodiment.Scope of the present invention is not subjected to the restriction of these embodiment, and scope of the present invention proposes in claims.
Embodiment 1～6:
With carbon black (carbon black ELFTEX TP, particle diameter≤25nm, U.S. CABOT company produces) and surface treatment agent (monoalkoxytitanates coupling agent, trade mark NDZ-101, Nanjing dawn Group Co.,Ltd produces) place homogenizer, 5min carries out the surface modification treatment of carbon black under 1500rpm stirs; Then with vector resin (new LDPE (film grade), trade mark 1F7B, the production of Beijing yanshan petrochemical limited-liability company of China Petrochemical Industry), carbon black and antioxidant 1010 (production of Switzerland vapour Ba Jiaji company), the oxidation inhibitor 168 (production of Switzerland vapour Ba Jiaji company) after the above-mentioned processing is put into Banbury mixer (GK type, Yiyang Rubber Plastics Machinery (Group) Co., Ltd. produces) in, start Banbury mixer, until the vector resin fusion, and and the mixed evenly back discharging of carbon black.Wherein the antioxidant 1010 consumption is 100 parts by weight in vector resin, is 0.2 part; Oxidation inhibitor 168 is 0.3 part.The material that is gone out placed in two roller mills be pressed into sheet material, the back pulverization process that cools, add then dispersion agent (1# polyethylene of dispersing agent wax, PEwax, 3 types, Beijing University of Chemical Technology produces; 2# dispersion agent ethylene bis stearamide EBS, the Shanghai Long March second chemical plant), obtains PE tubing with high heavy colour mother in twin screw extruder (the ZSK-25 twin screw extruder of WP company) melt blending extruding pelletization.And PE tubing base-material (the hdpe pipe base-material with prepared look female, trade mark 4803T, the limited production of sub-petrochemical complex share is raised by China Petrochemical Industry) in homogenizer after the simple and mechanical blend, at common polyolefin pipe extrusion equipment (PE (PP) 110 type tubing extrusion devices, Ningbo Fang Li company produces) upward extrusion moulding, gained tubing is carried out the test of carbon black dispersion degree by GB/T 18251-2000, carry out the test of carbon black content by GB/T 13021-1991.Concrete prescription and The performance test results are as shown in table 1.
Comparative Examples 1～2
Vector resin (new LDPE (film grade) is with embodiment 1), carbon black (with embodiment 1), antioxidant 1010 (vapour Bagong department) and oxidation inhibitor 168 (Ciba) are put into Banbury mixer.Start Banbury mixer, until the vector resin fusion, and and the mixed evenly back discharging of carbon black.Wherein the antioxidant 1010 consumption is 100 parts by weight in vector resin, is 0.2 part; Oxidation inhibitor 168 is 0.3 part.The material that is gone out placed in two roller mills be pressed into sheet material, the back pulverization process that cools, add then dispersion agent (1# polyethylene of dispersing agent wax, PEwax, 3 types, Beijing University of Chemical Technology produces; 2# dispersion agent ethylene bis stearamide (EBS), the Shanghai Long March second chemical plant) in twin screw extruder (with embodiment 1) melt blending extruding pelletization, prepare the carbon black masterbatch.Female and PE tubing base-material (with embodiment 1) is in homogenizer after the simple and mechanical blend with prepared look, extrusion moulding on common polyolefin pipe extrusion equipment, gained tubing carries out the test of carbon black dispersion degree by GB/T 18251-2000, carries out the test of carbon black content by GB/T 13021-1991.Concrete prescription and The performance test results are as shown in table 1.
Comparative Examples 3～4
Place homogenizer to carry out the surface modification treatment of carbon black carbon black (with embodiment 1) and surface treatment agent (dawn Group Co.,Ltd in Nanjing produces for monoalkoxytitanates coupling agent, trade mark NDZ-101); Then with the carbon black after vector resin (with embodiment 1), the processing, dispersion agent (1# polyethylene of dispersing agent wax, PEwax, 3 types, Beijing University of Chemical Technology's production; 2# dispersion agent EBS, the Shanghai Long March second chemical plant) and antioxidant 1010 (vapour Bagong department), oxidation inhibitor 168 (vapour Bagong department) put into Banbury mixer, start Banbury mixer, do not having to rely on self friction to heat up under the situation of indirect heating, until the vector resin fusion, and and the mixed evenly back discharging of carbon black.Wherein the antioxidant 1010 consumption is 100 parts by weight in vector resin, is 0.2 part; Oxidation inhibitor 168 is 0.3 part.The material that is gone out placed in two roller mills be pressed into sheet material, the back pulverization process that cools in twin screw extruder (with embodiment 1) melt blending extruding pelletization, is prepared the carbon black masterbatch then.Female and PE tubing base-material (with embodiment 1) is in homogenizer after the simple and mechanical blend with prepared look, extrusion moulding on common polyolefin pipe extrusion equipment, gained tubing carries out the test of carbon black dispersion degree by GB/T18251-2000, carries out the test of carbon black content by GB/T 13021-1991.Concrete prescription and The performance test results are as shown in table 1.
Table 1
| LDPE | Carbon black | NDZ-101 | PEwax | EBS | Look mother: PE4803T | Carbon black dispersion degree | Carbon black content | |
| Unit | Part | Part | Part | Part | Part | Amount ratio | Level | ％wt |
| Embodiment 1 | 100 | 80 | 5 | 6 | 6 | 1∶16 | 0.8 | 2.2 |
| Embodiment 2 | 100 | 100 | 5 | 8 | 4 | 1∶18 | 1.0 | 2.2 |
| Embodiment 3 | 100 | 120 | 5 | 6 | 6 | 1∶20 | 1.5 | 2.3 |
| Embodiment 4 | 100 | 120 | 10 | 6 | 6 | 1∶20 | 1.2 | 2.2 |
| Embodiment 5 | 100 | 140 | 8 | 8 | 8 | 1∶22 | 1.8 | 2.2 |
| Comparative Examples 1 | 100 | 100 | -- | 8 | 4 | 1∶18 | 3.3 | 2.3 |
| Comparative Examples 2 | 100 | 120 | -- | 6 | 6 | 1∶20 | 3.6 | 2.3 |
| Comparative Examples 3 | 100 | 100 | 5 | 8 | 4 | 1∶18 | 3.5 | 2.2 |
| Comparative Examples 4 | 100 | 120 | 5 | 6 | 6 | 1∶20 | 3.8 | 2.3 |
Comparative Examples 1～2 is not carried out surface treatment to carbon black, when the look mother of its preparation mixes with pipe resin in proportion, and behind extruding pipe material on the pipe extruder, records dispersity 〉=3 of carbon black, can not satisfy the requirement of relevant pipe workpiece quality standard.
In the Comparative Examples 3～4, just dispersion agent is put in the Banbury mixer in the banburying stage, rather than such with what mention among the embodiment, dispersion agent is to add in the screw mixes stage again, prepared look mother's dispersion effect is also undesirable, can not satisfy the requirement of relevant pipe workpiece quality standard.
Claims (10)
1. color masterbatch for polythene includes the following component of blend:
A. vector resin 100 parts by weight
B. carbon black 40～180 parts by weight
C. surface treatment agent 0.5～20 parts by weight
D. dispersion agent 1～20 parts by weight
The vector resin of the above component a comprises polyvinyl resin, ethylene-vinyl acetate copolymer or its mixing; The carbon black median size of described components b is 10～30nm; The surface treatment agent of described amount of component b comprises at least a in the following material: titanate coupling agent, aluminate coupling agent, silane coupling agent, soap or stearate; The dispersion agent of described component d comprises at least a in the following material: oxidic polyethylene, polyethylene wax, stearic acid, stearate, solid paraffin, whiteruss, dioctyl phthalate (DOP), turps, triphenylphosphate or ethylene bis stearamide.
2. color masterbatch for polythene according to claim 1 includes the following component of blend:
A. vector resin 100 parts by weight
B. carbon black 80～150 parts by weight
C. surface treatment agent 1～10 parts by weight
D. dispersion agent 5～15 parts by weight
3. color masterbatch for polythene according to claim 1, wherein the vector resin of component a is a new LDPE (film grade).
4. color masterbatch for polythene according to claim 1, wherein the median size of the carbon black of components b is 15～25nm.
5. color masterbatch for polythene according to claim 1, wherein the surface treatment agent of amount of component b is a titanate coupling agent.
6. color masterbatch for polythene according to claim 1, wherein the dispersion agent of component d comprises at least a in the following material: polyethylene wax, stearic acid or ethylene bis stearamide.
7. according to each described color masterbatch for polythene of claim 1～6, it is prepared by the method that may further comprise the steps:
1. described carbon black and surface treatment agent are pressed the even blend of described consumption;
2. will comprise the step 1. carbon black handled of surface treatment agent, component banburying in Banbury mixer of described vector resin, mix, after the discharging, compressing tablet, pulverizing;
3. with step 2. after the pulverizing material of gained and the described dispersant melt blending obtain described color masterbatch for polythene.
8. preparation method according to each described color masterbatch for polythene of claim 1～6 may further comprise the steps:
1. described carbon black and surface treatment agent are pressed the even blend of described consumption;
2. will comprise the step 1. carbon black handled of surface treatment agent, component banburying in Banbury mixer of described vector resin, mix, after the discharging, compressing tablet, pulverizing;
3. with step 2. after the pulverizing material of gained and the described dispersant melt blending obtain described color masterbatch for polythene.
9. the preparation method of color masterbatch for polythene according to claim 8, wherein step mixes surface treatment agent and carbon black by high-speed stirring in 1..
10. the preparation method of color masterbatch for polythene according to claim 8, wherein step utilizes screw extrusion press that described material is carried out melt blending in 3., and the melt blending temperature is 60～180 ℃.
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