CN110606903A - Chlorinated linear low-density polyethylene and preparation method thereof - Google Patents
Chlorinated linear low-density polyethylene and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of high polymer materials, in particular to chlorinated linear low-density polyethylene and a preparation method thereof, wherein the chlorinated linear low-density polyethylene comprises the following components: linear low-density polyethylene, a molecular weight regulator, a lubricant, an antioxidant, an emulsifier, an opening agent, an antistatic agent, a dispersant A, a dispersant B, an anti-sticking agent, an initiator A, an initiator B, process water and chlorine, wherein the components in parts by weight are respectively as follows: the invention reduces corrosion rate and improves comprehensive properties such as reaction pressure, hardness, fracture resistance, toughness and the like by designing chlorinated linear low-density polyethylene and can meet the requirements of current life.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to chlorinated linear low-density polyethylene and a preparation method thereof.
Background
Chlorinated Polyethylene (CPE) is a modified polymer prepared by chlorination substitution reaction of High Density Polyethylene (HDPE), and is generally prepared from the high density polyethylene with the density range of 0.93-0.96g/cm3, the average molecular weight of 5-25 ten thousand and the melt index of 0.01-2.0g/10 min. It is an excellent impact modifier for PVC plastics, and is also a synthetic rubber with good performance, such as amorphous structure saturated special rubber (CM) with 25-45 parts of chlorine content, which is widely used for products such as cables, wires, rubber tubes, rubberized fabrics, rubber and plastic products, sealing materials, flame-retardant conveyor belts, waterproof coiled materials, films and various profiled bars. The corrosion rate and reaction pressure of the existing chlorinated linear low-density polyethylene, and the comprehensive properties of hardness, fracture resistance, toughness and the like can not meet the requirements of the current life.
In summary, the present invention provides a chlorinated linear low density polyethylene and a preparation method thereof to solve the existing problems
Disclosure of Invention
The present invention is directed to a chlorinated linear low density polyethylene and a method for preparing the same, which solves the problems set forth in the background art.
In order to achieve the purpose, the invention provides the following technical scheme:
a chlorinated linear low density polyethylene comprising the following components: linear low-density polyethylene, a molecular weight regulator, a lubricant, an antioxidant, an emulsifier, an opening agent, an antistatic agent, a dispersant A, a dispersant B, an anti-sticking agent, an initiator A, an initiator B, process water and chlorine, wherein the components in parts by weight are respectively as follows: 10-15 parts of linear low-density polyethylene, 2-3 parts of molecular weight regulator, 2-3 parts of lubricant, 7-9 parts of antioxidant, 6-7 parts of emulsifier, 3-4 parts of opening agent, 2-3 parts of antistatic agent, 1-2 parts of dispersant A, 2-3 parts of dispersant B, 1-2 parts of anti-sticking agent, 1-2 parts of initiator A, 2-3 parts of initiator B, 2-3 parts of stabilizer, 60-65 parts of process water and 10-15 parts of chlorine.
Preferably, the linear low-density polyethylene is 200-mesh 300-mesh powdery solid, the process water is deionized water, the molecular weight regulator is propylene or propane or hexane, the antioxidant is 4-methyl-2, 6-di-tert-butylphenol, the lubricant is a mixture of oleamide or ammonium stearate, ammonium oleate and ammonium linseed oil as a polyethylene lubricant, the opening agent is high-dispersion silica gel, alumina gel or a mixture thereof as an opening agent, and the antistatic agent is a polymer containing amino or alkyl and other machine type groups.
Preferably, the dispersant A is pyrrolidone, and the dispersant B is special silicon dioxide; the anti-sticking agent is light calcium carbonate, the initiator A is peroxide, the initiator B is azo series, the emulsifier is castor oil polyoxyethylene ether series, the dispersant A is sodium dodecyl benzene sulfonate or sodium dodecyl sulfate, the dispersant B is organic silicon treated superfine white carbon black, and the anti-sticking agent is calcium stearate, light calcium carbonate or heavy calcium carbonate.
Preferably, the method comprises the following steps:
s1, selecting the following raw materials: linear low-density polyethylene, a molecular weight regulator, a lubricant, an antioxidant, an emulsifier, an opening agent, an antistatic agent, a dispersant A, a dispersant B, an anti-sticking agent, an initiator A, an initiator B, process water and chlorine;
s2, weighing the following components in parts by weight: 10-15 parts of linear low-density polyethylene, 2-3 parts of molecular weight regulator, 2-3 parts of lubricant, 7-9 parts of antioxidant, 6-7 parts of emulsifier, 3-4 parts of opening agent, 2-3 parts of antistatic agent, 1-2 parts of dispersant A, 2-3 parts of dispersant B, 1-2 parts of anti-sticking agent, 1-2 parts of initiator A, 2-3 parts of initiator B, 2-3 parts of stabilizer, 60-65 parts of process water and 10-15 parts of chlorine;
s3, adding 60-65 parts of process water into an emulsifying kettle, starting a stirrer and stirring at a certain stirring speed, slowly adding 6-7 parts of emulsifier, 1-2 parts of dispersant A, 2-3 parts of dispersant B and 1-2 parts of anti-sticking agent, adding 10-15 parts of linear low-density polyethylene, heating the materials in the emulsifying kettle after the materials become suspension, discharging the materials to a chlorination kettle while stirring, and continuing for a period of time;
s4, starting a stirrer of the chlorination kettle, stirring S3 to obtain a material, adding 1-2 parts of an initiator A and 2-3 parts of an initiator B, sealing the chlorination kettle, heating to 120 ℃ after 100-;
s5, conveying the materials in the chlorination kettle to a deacidification washing tank through compressed air, washing the materials in the deacidification washing tank after solid-liquid separation for a period of time, pumping the materials into a neutralization tank by a pump, heating the materials in the neutralization tank under stirring, adding alkali to reach a certain PH value, continuing for a period of time, cooling to wash the alkali, and pumping the materials into a dealkalization kettle by a pump.
S6, further cooling the material under the stirring condition of a dealkalization kettle, dealkalizing and centrifuging after cooling, pumping the material passing through a filter screen through a horizontal spiral sedimentation type centrifuge to remove process water, adding 2-3 parts of a molecular weight regulator, 2-3 parts of a lubricant, 7-9 parts of an antioxidant, 6-7 parts of an emulsifier, 3-4 parts of an opening agent and 2-3 parts of an antistatic agent into the centrifuged material, and finally adding 2-3 parts of a stabilizer into the mixer for stirring;
and S7, mixing, drying by a dryer set, centrifuging, drying, sieving and packaging to obtain the finished product.
Preferably, the stirring speed of the stirrer in the S3 is 500-600 rpm/min, the temperature is increased and heated to 75-90 ℃, and the time is 80-90 minutes.
Preferably, the washing in S5 is performed at least 4 times and each time lasts for 30-40 minutes, the pH is 8.5-9 and lasts for 140-160 minutes, and the neutralization tank is 10-20m3And (3) a neutralization tank for the polyhexene material, and heating to 50-70 ℃ under stirring.
Preferably, the temperature of the S6 is reduced to 20-30 ℃ for 80-100 minutes, the time for removing the process water by the centrifuge is 80-90 minutes, and the time for centrifuging and drying in the S7 is 200-250 minutes.
Compared with the prior art, the invention has the beneficial effects that:
1. in the invention, the molecular weight regulator, the lubricant, the antioxidant and the opening agent are designed to be strictly proportioned in the preparation process of the linear low density polyethylene by taking the molecular weight regulator, the lubricant, the antioxidant and the opening agent as additives, so that the corrosion rate of chlorinated linear low density polyethylene is reduced, and the service life of the linear low density polyethylene is prolonged.
2. In the invention, by designing the strict proportion among the components of the raw materials and carrying out comparison and detection, the comprehensive properties of the chlorinated linear low-density polyethylene such as hardness, fracture resistance, toughness and the like are improved compared with the traditional chlorinated polyethylene, thereby meeting the current requirements.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, rather than all embodiments, and all other embodiments obtained by those skilled in the art without any creative work based on the embodiments of the present invention belong to the protection scope of the present invention.
The invention provides a technical scheme that:
a chlorinated linear low density polyethylene comprising the following components: linear low-density polyethylene, a molecular weight regulator, a lubricant, an antioxidant, an emulsifier, an opening agent, an antistatic agent, a dispersant A, a dispersant B, an anti-sticking agent, an initiator A, an initiator B, process water and chlorine, wherein the components in parts by weight are respectively as follows: 10-15 parts of linear low-density polyethylene, 2-3 parts of molecular weight regulator, 2-3 parts of lubricant, 7-9 parts of antioxidant, 6-7 parts of emulsifier, 3-4 parts of opening agent, 2-3 parts of antistatic agent, 1-2 parts of dispersant A, 2-3 parts of dispersant B, 1-2 parts of anti-sticking agent, 1-2 parts of initiator A, 2-3 parts of initiator B, 2-3 parts of stabilizer, 60-65 parts of process water and 10-15 parts of chlorine.
Example 1:
step 1, selecting a chlorinated linear low-density polyethylene preparation material, and weighing the materials according to the weight percentage: 10 parts of linear low-density polyethylene, 2 parts of molecular weight regulator, 2 parts of lubricant, 7 parts of antioxidant, 6 parts of emulsifier, 3 parts of opening agent, 2 parts of antistatic agent, 1 part of dispersant A, 2 parts of dispersant B, 1 part of anti-sticking agent, 1 part of initiator A, 2 parts of initiator B, 2 parts of stabilizer, 60 parts of process water and 10 parts of chlorine;
step 2, adding 60 parts of process water into an emulsifying kettle after metering, starting a stirrer, slowly adding 6 parts of emulsifier, 1 part of dispersant A, 2 parts of dispersant B and 1 part of anti-sticking agent at the stirring speed of the stirrer of 500-600 rpm/min, adding 10 parts of linear low density polyethylene, heating the emulsifying kettle materials to 75 ℃ after the emulsifying kettle materials become suspension, discharging the materials into a chlorination kettle while stirring, and continuing for 80-90 minutes;
step 3, starting a chlorination kettle stirrer, stirring the materials generated in the step 2, adding 1 part of initiator A and 2 parts of initiator B, sealing the chlorination kettle, heating to 120 ℃ of 100 plus materials, introducing 10 parts of chlorine gas at 500-550 liters per hour for reaction, carrying out chlorination reaction for 45-60 minutes, discharging residual chlorine gas in the chlorination kettle into a tail gas absorption system after the reaction is finished, introducing compressed air into the chlorination kettle to replace residual chlorine gas in the chlorination kettle, and pressing the materials into a deacidification washing tank;
and 4, pumping the materials in the chlorination reaction kettle to a deacidification washing tank through compressed air, washing the process water for at least 4 times after solid-liquid separation and lasting for 30-40 minutes each time, pumping the materials into a neutralization tank by using a pump, heating the materials in the neutralization tank to 50-70 ℃ under stirring, adding alkali to a certain pH value of 8.5 and lasting for 160 minutes, cooling and washing the alkali, and pumping the materials into a dealkalization kettle by using a pump.
Step 5, further cooling the material to 20-30 ℃ under the stirring condition of a dealkalization kettle, cooling to 20-30 ℃ for 80-100 minutes, dealkalizing and centrifuging, pumping the material passing through a filter screen through a horizontal spiral sedimentation type centrifuge to remove process water, dewatering for 80-90 minutes, respectively adding 2 parts of molecular weight regulator, 2 parts of lubricant, 7 parts of antioxidant, 6 parts of emulsifier, 3 parts of opening agent and 2 parts of antistatic agent into the centrifuged material, and finally adding 2 parts of stabilizer into the mixing interior of a mixer to stir;
and 6, drying the mixture by using a drying unit after mixing, centrifuging and drying for 200 and 250 minutes, and sieving and packaging to obtain a finished product.
Example 2:
step 1, selecting a chlorinated linear low-density polyethylene preparation material, and weighing the materials according to the weight percentage: 12 parts of linear low-density polyethylene, 2.5 parts of molecular weight regulator, 2.5 parts of lubricant, 8 parts of antioxidant, 6.5 parts of emulsifier, 3.5 parts of opening agent, 2.5 parts of antistatic agent, 1.5 parts of dispersant A, 2.5 parts of dispersant B, 1.5 parts of anti-sticking agent, 1.5 parts of initiator A, 2.5 parts of initiator B, 2.5 parts of stabilizer, 63 parts of process water and 12 parts of chlorine;
step 2, metering 63 parts of process water, then adding the process water into an emulsifying kettle, starting a stirrer, slowly adding 6.5 parts of emulsifier, 1.5 parts of dispersant A, 2.5 parts of dispersant B and 1.5 parts of anti-sticking agent at the stirring speed of the stirrer, then adding 12 parts of linear low-density polyethylene, heating the emulsifying kettle material to 75-90 ℃ after the emulsifying kettle material becomes suspension, discharging the material into a chlorination kettle while stirring, and continuing for 80-90 minutes;
step 3, starting a chlorination kettle stirrer, stirring the materials generated in the step 2, adding 1.5 parts of initiator A and 2.5 parts of initiator B, sealing the chlorination kettle, heating to 120 ℃ for 100 plus materials, introducing 12 parts of chlorine gas at 500-550 liters per hour for reaction, carrying out chlorination reaction for 45-60 minutes, discharging residual chlorine gas in the chlorination kettle into a tail gas absorption system after the reaction is finished, introducing compressed air into the chlorination kettle to replace residual chlorine gas in the chlorination kettle, and pressing the materials into a deacidification washing tank;
and 4, pumping the materials in the chlorination reaction kettle to a deacidification washing tank through compressed air, washing the process water for at least 4 times after solid-liquid separation and lasting for 30-40 minutes each time, pumping the materials into a neutralization tank by using a pump, heating the materials in the neutralization tank to 50-70 ℃ under stirring, adding alkali to a certain pH value of 8.8 and lasting for 160 minutes, cooling and washing the alkali, and pumping the materials into a dealkalization kettle by using a pump.
Step 5, further cooling the material to 20-30 ℃ under the stirring condition of a dealkalization kettle, cooling to 20-30 ℃ for 80-100 minutes, dealkalizing and centrifuging, pumping the material passing through a filter screen through a horizontal spiral sedimentation type centrifuge to remove process water, dewatering for 80-90 minutes, respectively adding 2.5 parts of molecular weight regulator, 2.5 parts of lubricant, 8 parts of antioxidant, 6.5 parts of emulsifier, 3.5 parts of opening agent and 2.5 parts of antistatic agent into the centrifuged material, and finally adding 2.5 parts of stabilizer into the mixer for stirring;
and 6, drying the mixture by using a drying unit after mixing, sieving and packaging the mixture after centrifuging and drying for 200-250 minutes to obtain a finished product, and detecting the finished product by using a detection instrument.
Example 3:
step 1, selecting a chlorinated linear low-density polyethylene preparation material, and weighing the materials according to the weight percentage: 15 parts of linear low-density polyethylene, 3 parts of molecular weight regulator, 3 parts of lubricant, 9 parts of antioxidant, 7 parts of emulsifier, 4 parts of opening agent, 3 parts of antistatic agent, 2 parts of dispersant A, 3 parts of dispersant B, 2 parts of anti-sticking agent, 2 parts of initiator A, 3 parts of initiator B, 3 parts of stabilizer, 65 parts of process water and 15 parts of chlorine;
step 2, adding 65 parts of process water into an emulsifying kettle after metering, starting the stirrer, slowly adding 7 parts of emulsifier, 2 parts of dispersant A, 3 parts of dispersant B and 2 parts of anti-sticking agent at the stirring speed of the stirrer of 500-600 rpm/min, then adding 15 parts of linear low density polyethylene, heating the emulsifying kettle material to 75-90 ℃ after the emulsifying kettle material becomes suspension, discharging the suspension to a chlorination kettle while stirring, and continuing for 80-90 minutes;
step 3, starting a chlorination kettle stirrer, stirring the materials generated in the step 2, adding 2 parts of initiator A and 3 parts of initiator B, sealing the chlorination kettle, heating to 120 ℃ of 100 plus materials, introducing 15 parts of chlorine gas at 500-550 liters per hour for reaction, carrying out chlorination reaction for 45-60 minutes, discharging residual chlorine gas in the chlorination kettle into a tail gas absorption system after the reaction is finished, introducing compressed air into the chlorination kettle to replace residual chlorine gas in the chlorination kettle, and pressing the materials into a deacidification washing tank;
and 4, pumping the materials in the chlorination reaction kettle to a deacidification washing tank through compressed air, washing the process water for at least 4 times after solid-liquid separation and lasting for 30-40 minutes each time, pumping the materials into a neutralization tank by using a pump, heating the materials in the neutralization tank to 50-70 ℃ under stirring, adding alkali to a certain pH value of 9 and lasting for 160 minutes for 140 and alkali washing, cooling and alkali washing, and pumping the materials into a dealkalization kettle by using a pump.
Step 5, further cooling the material to 20-30 ℃ under the stirring condition of a dealkalization kettle, cooling to 20-30 ℃ for 80-100 minutes, dealkalizing and centrifuging, pumping the material passing through a filter screen through a horizontal spiral sedimentation type centrifuge to remove process water, dewatering for 80-90 minutes, respectively adding 3 parts of molecular weight regulator, 3 parts of lubricant, 9 parts of antioxidant, 7 parts of emulsifier, 4 parts of opening agent and 3 parts of antistatic agent into the centrifuged material, and finally adding 3 parts of stabilizer into the mixing interior of a mixer to stir;
and 6, drying the mixture by using a drying unit after mixing, centrifuging and drying for 200 and 250 minutes, and sieving and packaging to obtain a finished product.
The chlorinated linear low-density polyethylene formed by matching in the embodiment 1, 2 and 3 is detected by an experimental instrument and compared with the chlorinated linear low-density polyethylene obtained by matching the components in the embodiment 2 according to the detected data, so that the corrosion rate is reduced, and the comprehensive performances such as reaction pressure, hardness, fracture resistance, toughness and the like are improved more remarkably.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (7)
1. A chlorinated linear low density polyethylene comprising the following components: linear low-density polyethylene, a molecular weight regulator, a lubricant, an antioxidant, an emulsifier, an opening agent, an antistatic agent, a dispersant A, a dispersant B, an anti-sticking agent, an initiator A, an initiator B, process water and chlorine, wherein the components in parts by weight are respectively as follows: 10-15 parts of linear low-density polyethylene, 2-3 parts of molecular weight regulator, 2-3 parts of lubricant, 7-9 parts of antioxidant, 6-7 parts of emulsifier, 3-4 parts of opening agent, 2-3 parts of antistatic agent, 1-2 parts of dispersant A, 2-3 parts of dispersant B, 1-2 parts of anti-sticking agent, 1-2 parts of initiator A, 2-3 parts of initiator B, 2-3 parts of stabilizer, 60-65 parts of process water and 10-15 parts of chlorine.
2. The chlorinated linear low density polyethylene as claimed in claim 1, wherein the linear low density polyethylene is 200-300 mesh powder solid, the process water is deionized water, the molecular weight regulator is propylene or propane or hexane, the antioxidant is 4-methyl-2, 6-di-tert-butylphenol, the lubricant is mixture of oleamide or ammonium stearate, ammonium oleate and ammonium linseed oil as the lubricant of polyethylene, the opening agent is highly dispersed silica gel, aluminum gel or mixture thereof as opening agent, and the antistatic agent is polymer containing amino or alkyl group.
3. The chlorinated linear low density polyethylene according to claim 1, wherein the dispersant a is pyrrolidone, the dispersant B is special silica; the anti-sticking agent is light calcium carbonate, the initiator A is peroxide, the initiator B is azo series, the emulsifier is castor oil polyoxyethylene ether series, the dispersant A is sodium dodecyl benzene sulfonate or sodium dodecyl sulfate, the dispersant B is organic silicon treated superfine white carbon black, and the anti-sticking agent is calcium stearate, light calcium carbonate or heavy calcium carbonate.
4. A method for preparing chlorinated linear low density polyethylene is characterized by comprising the following steps:
s1, selecting the following raw materials: linear low-density polyethylene, a molecular weight regulator, a lubricant, an antioxidant, an emulsifier, an opening agent, an antistatic agent, a dispersant A, a dispersant B, an anti-sticking agent, an initiator A, an initiator B, process water and chlorine;
s2, weighing the following components in parts by weight: 10-15 parts of linear low-density polyethylene, 2-3 parts of molecular weight regulator, 2-3 parts of lubricant, 7-9 parts of antioxidant, 6-7 parts of emulsifier, 3-4 parts of opening agent, 2-3 parts of antistatic agent, 1-2 parts of dispersant A, 2-3 parts of dispersant B, 1-2 parts of anti-sticking agent, 1-2 parts of initiator A, 2-3 parts of initiator B, 2-3 parts of stabilizer, 60-65 parts of process water and 10-15 parts of chlorine;
s3, adding 60-65 parts of process water into an emulsifying kettle, starting a stirrer and stirring at a certain stirring speed, slowly adding 6-7 parts of emulsifier, 1-2 parts of dispersant A, 2-3 parts of dispersant B and 1-2 parts of anti-sticking agent, adding 10-15 parts of linear low-density polyethylene, heating the materials in the emulsifying kettle after the materials become suspension, discharging the materials to a chlorination kettle while stirring, and continuing for a period of time;
s4, starting a stirrer of the chlorination kettle, stirring S3 to obtain a material, adding 1-2 parts of an initiator A and 2-3 parts of an initiator B, sealing the chlorination kettle, heating to 120 ℃ after 100-;
s5, conveying the materials in the chlorination kettle to a deacidification washing tank through compressed air, washing the materials in the deacidification washing tank after solid-liquid separation for a period of time, pumping the materials into a neutralization tank by a pump, heating the materials in the neutralization tank under stirring, adding alkali to reach a certain PH value, continuing for a period of time, cooling to wash the alkali, and pumping the materials into a dealkalization kettle by a pump.
S6, further cooling the material under the stirring condition of a dealkalization kettle, dealkalizing and centrifuging after cooling, pumping the material passing through a filter screen through a horizontal spiral sedimentation type centrifuge to remove process water, adding 2-3 parts of a molecular weight regulator, 2-3 parts of a lubricant, 7-9 parts of an antioxidant, 6-7 parts of an emulsifier, 3-4 parts of an opening agent and 2-3 parts of an antistatic agent into the centrifuged material, and finally adding 2-3 parts of a stabilizer into the mixer for stirring;
and S7, mixing, drying by a dryer set, centrifuging, drying, sieving and packaging to obtain the finished product.
5. The method of claim 4, wherein the stirring speed of the stirrer in S3 is 500-600 rpm/min, the temperature rise is 75-90 ℃, and the time is 80-90 minutes.
6. The method as claimed in claim 4, wherein the S5 is washed at least 4 times for 30-40 min each, the pH is 8.5-9 for 140-160 min, and the neutralization tank is 10-20m3And (3) a neutralization tank for the polyhexene material, and heating to 50-70 ℃ under stirring.
7. The method as claimed in claim 4, wherein the temperature of S6 is reduced to 20-30 ℃ for 80-100 min, the time for removing process water by the centrifuge is 80-90 min, and the time for centrifuging and drying in S7 is 200-250 min.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102690382A (en) * | 2012-06-14 | 2012-09-26 | 江苏中煦高分子材料有限公司 | Linear low density polyethylene synthesis process by means of chlorination through aqueous suspension method |
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| CN103930449A (en) * | 2011-11-07 | 2014-07-16 | 株式会社钟化 | Method for producing chlorinated vinyl chloride resin |
| CN102690382A (en) * | 2012-06-14 | 2012-09-26 | 江苏中煦高分子材料有限公司 | Linear low density polyethylene synthesis process by means of chlorination through aqueous suspension method |
| CN104650473A (en) * | 2013-11-25 | 2015-05-27 | 江苏中煦高分子材料有限公司 | Chlorinated polyethylene rubber produced by water phase suspension method and synthesis technology thereof |
| CN104650271A (en) * | 2013-11-25 | 2015-05-27 | 江苏中煦高分子材料有限公司 | Chlorinated ultra-low density polyethylene produced by water phase suspension method and synthesis technology thereof |
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