CN102690382A - Linear low density polyethylene synthesis process by means of chlorination through aqueous suspension method - Google Patents
Linear low density polyethylene synthesis process by means of chlorination through aqueous suspension method Download PDFInfo
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- CN102690382A CN102690382A CN2012101961172A CN201210196117A CN102690382A CN 102690382 A CN102690382 A CN 102690382A CN 2012101961172 A CN2012101961172 A CN 2012101961172A CN 201210196117 A CN201210196117 A CN 201210196117A CN 102690382 A CN102690382 A CN 102690382A
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Abstract
The invention discloses a linear low density polyethylene synthesis process by means of chlorination through aqueous suspension method, which includes the following steps of: step1, putting process water into an chlorination reactor, putting emulsifier, dispersing agent(A), dispersing agent(B) and antiseize compound into the reactor, finally putting linear low density polyethylene into the reactor, and stirring while putting the materials into the chlorination reactor; step 2, stirring the materials obtained from step1, adding initiator into the mixture and introducing chlorine to react; step3, compressing the materials in the chlorination reactor to a deacidification washing tank, and then throwing the materials into a neutralizing tank; step 4, adding alkali to neutralize the materials until the pH value reaches 8-10, cooling, lixiviating and then throwing the materials into a dealkalization kettle; step 5, stirring the materials in the dealkalization kettle to further cool the materials, and after 60-80mins, dealkalizing and centrifuging the materials; step 6, removing the process water through a centrifuge; step 7, adding antiseize compound into the centrifuged materials and drying; and step 8, sieving and packaging to obtain a finished product. The synthesis process is high in automation level of control and the work intensity is reduced.
Description
Technical field
The present invention relates to water phase suspension chlorination LLDPE synthesis technique.
Background technology
Chlorinatedpolyethylene (be called for short CPE, CM) is by high density polyethylene(HDPE) (0.941～0.970g/cm3) product that makes at aqueous phase and chlorine reaction.It is a kind of special synthetic rubber, is again a kind of good plastic modifier.In October, 1973, Anhui Chemical Engineering Inst. began the research with water phase suspension chlorinatedpolyethylene technology; 06 month nineteen eighty-three, the kiloton industrialized unit built up; In November, 1984 is through two innings of technical evaluation of the Ministry of Chemical Industry; China's ultimate production is (wherein CPE output is that 400,000 tons, CM output are 100,000 tons) more than 500,000 tons now, is 7～8 times of Gross World Product.About 40 families of present national factory; Product is carried out chemical industry standard HG/T2704-2010; Along with having driven the chlorinated polyethylene rubber market requirement, China's rubber industry fast development sharply increases; Simultaneously because China's quality certification system, constantly improve the generally increase with enterprise-quality consciousness, market is also increasingly high to the requirement of the quality of CM, brand; Simply, the incompatibility rubber industry development of extensive style, single CM product, be badly in need of to chlorinated polyethylene rubber (CM) product carry out perfect, transform, innovation.
Summary of the invention
The present invention is directed to the problem in the background technology, researched and developed water phase suspension chlorination LLDPE synthesis technique, purpose is: improve product quality and production efficiency.
Technical solution of the present invention:
Water phase suspension chlorination LLDPE synthesis technique, concrete steps are:
Step 1: the emulsification still is dropped in process water metering back; Open and stir; Drop into emulsifying agent, dispersion agent (A), dispersion agent (B) and release agent earlier, drop into LLDPE again, intensification was heated to 30～100 ℃ after emulsification still material became suspension-s; Be discharged to chlorination tank while stirring, the time was controlled at 60～80 minutes.
Step 2: open the chlorination tank stirrer, the material that whipping step one generates adds initiator then; Airtight chlorination tank also is warming up to 30～150 ℃, feeds chlorine again and reacts, and stops logical chlorine reach 1 to 1.4 times of polyethylene powder when logical chlorine dose after; 150～300 minutes chlorination reaction time, after reaction finishes, more remaining chlorine in the still is entered the tail gas absorption system; In still, feed afterwards in the pressurized air displacement still and remain chlorine, again material is pressed into the depickling rinse bath.
Step 3: material in the chlorination reaction still is depressed into the depickling rinse bath through pressurized air, and the process water washing is 2～8 times after the solid-liquid separation, and time control 80～110 minutes is squeezed into neutralizing well
with material with pump then.
Step 4: the material in the neutralizing well under agitation is warming up to 40～100 ℃, adds alkali then and be neutralized to pH value 8～10 and kept 120～200 minutes, the soda of lowering the temperature is afterwards squeezed into the dealkalize still with pump again.
Step 5: material is further cooling under dealkalize still agitation condition, dealkalize and centrifugal after 60～80 minutes.
Step 6: squeeze into whizzer through the material of filtering net through pump and slough process water, time control 60～80 minutes.
Step 7: material adds release agent and dry after centrifugal, centrifugal and 200 minutes time of drying.
Step 8: dry back material is added thermo-stabilizer, and the packing of after blender mixes 40～70 minutes, sieving gets product.
Process water in the said step 1 is deionized water or tap water.
Chlorine feeding speed in the said step 2 is 400～600 liter liquid per hour.
Chlorine feeding amount adopts the control of DCS robot control system(RCS) in the said step 2.
Neutralizing well in the said step 3 is the neutralizing well of 15m3 Vestolen PP 7052 material.
Whizzer in the said step 6 adopts PTM type decaner.
Drying process in the said step 7 adopts air-flow to add 8 ㎡ fluidized drying units.
Said emulsifying agent in the above-mentioned steps is the epoxy Viscotrol C; Dispersion agent (A) is a pyrrolidone; Dispersion agent (B) is a special silica; Release agent is a light calcium carbonate; Initiator is a superoxide.
Beneficial effect of the present invention:
The automatization level height of this technological process control not only improves operating environment, and reduces labor intensity, and reduces corrosion rate and reaction kettle pressure simultaneously greatly, and aftertreatment adopts the Vestolen PP 7052 neutralizing well effectively to improve the quality of products.
Description of drawings
Accompanying drawing is a process flow diagram of the present invention.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is further specified.
Accompanying drawing is a process flow diagram of the present invention:
Step 1: deionized water or tap water metering back are dropped into the emulsification still; Open and stir; Drop into emulsifying agent, dispersion agent (A), dispersion agent (B) and release agent earlier, drop into LLDPE again, intensification was heated to 30～100 ℃ after emulsification still material became suspension-s; Be discharged to chlorination tank while stirring, the time was controlled at 60～80 minutes.
Step 2: open the chlorination tank stirrer, the material that whipping step one generates adds initiator then; Airtight chlorination tank also is warming up to 30～150 ℃, feeds chlorine again and reacts, and chlorine feeding speed is 400～600 liters per hour; Adopt the control of DCS robot control system(RCS), stop logical chlorine, 150～300 minutes chlorination reaction time reach 1 to 1.4 times of polyethylene powder when logical chlorine dose after; After reaction finishes; Again remaining chlorine in the still is entered the tail gas absorption system, in still, feed afterwards in the pressurized air displacement still and remain chlorine, again material is pressed into the depickling rinse bath.
Step 3: material in the chlorination reaction still is depressed into the depickling rinse bath through pressurized air, and the process water washing is 2～8 times after the solid-liquid separation, and the time is controlled 80～110 minutes, then material is squeezed into the neutralizing well
of 15m3 Vestolen PP 7052 material with pump.
Step 4: the material in the neutralizing well under agitation is warming up to 40～100 ℃, adds alkali then and be neutralized to pH value 8～10 and kept 120～200 minutes, the soda of lowering the temperature is afterwards squeezed into the dealkalize still with pump again.
Step 5: material is further cooling under dealkalize still agitation condition, dealkalize and centrifugal after 60～80 minutes.
Step 6: squeeze into PTM type decaner through the material of filtering net through pump and slough process water, time control 60～80 minutes.
Step 7: material adds release agent after centrifugal, uses air-flow to add 8 ㎡ fluidized drying units then and carries out drying, centrifugal and 200 minutes time of drying.
Step 8: dry back material is added thermo-stabilizer, and the packing of after blender mixes 40～70 minutes, sieving gets product.
Claims (8)
1. water phase suspension chlorination LLDPE synthesis technique, concrete steps are:
Step 1: the emulsification still is dropped in process water metering back; Open and stir; Drop into emulsifying agent, dispersion agent (A), dispersion agent (B) and release agent earlier, drop into LLDPE again, intensification was heated to 30～100 ℃ after emulsification still material became suspension-s; Be discharged to chlorination tank while stirring, the time was controlled at 60～80 minutes;
Step 2: open the chlorination tank stirrer, the material that whipping step one generates adds initiator then; Airtight chlorination tank also is warming up to 30～150 ℃, feeds chlorine again and reacts, and stops logical chlorine reach 1 to 1.4 times of polyethylene powder when logical chlorine dose after; 150～300 minutes chlorination reaction time, after reaction finishes, more remaining chlorine in the still is entered the tail gas absorption system; In still, feed afterwards in the pressurized air displacement still and remain chlorine, again material is pressed into the depickling rinse bath;
Step 3: material in the chlorination reaction still is depressed into the depickling rinse bath through pressurized air, and the process water washing is 2～8 times after the solid-liquid separation, and time control 80～110 minutes is squeezed into neutralizing well with material with pump then
Step 4: the material in the neutralizing well under agitation is warming up to 40～100 ℃, adds alkali then and be neutralized to pH value 8～10 and kept 120～200 minutes, the soda of lowering the temperature is afterwards squeezed into the dealkalize still with pump again;
Step 5: material is further cooling under dealkalize still agitation condition, dealkalize and centrifugal after 60～80 minutes;
Step 6: squeeze into whizzer through the material of filtering net through pump and slough process water, time control 60～80 minutes;
Step 7: material adds release agent and dry after centrifugal, centrifugal and 200 minutes time of drying;
Step 8: dry back material is added thermo-stabilizer, and the packing of after blender mixes 40～70 minutes, sieving gets product.
2. water phase suspension chlorination LLDPE synthesis technique as claimed in claim 1, it is characterized in that: the process water in the said step 1 is deionized water or tap water.
3. water phase suspension chlorination LLDPE synthesis technique as claimed in claim 1 is characterized in that: the chlorine feeding speed in the said step 2 is 400～600 liter liquid per hour.
4. water phase suspension chlorination LLDPE synthesis technique as claimed in claim 1 is characterized in that: chlorine feeding amount adopts the control of DCS robot control system(RCS) in the said step 2.
5. water phase suspension chlorination LLDPE synthesis technique as claimed in claim 1, it is characterized in that: the neutralizing well in the said step 3 is the neutralizing well of 15m3 Vestolen PP 7052 material.
6. water phase suspension chlorination LLDPE synthesis technique as claimed in claim 1 is characterized in that: the whizzer in the said step 6 adopts PTM type decaner.
7. water phase suspension chlorination LLDPE synthesis technique as claimed in claim 1 is characterized in that: the drying process in the said step 7 adopts air-flow to add 8 ㎡ fluidized drying units.
8. a kind of chlorination LLDPE as claimed in claim 1 is characterized in that: the said emulsifying agent in the above-mentioned steps is the epoxy Viscotrol C; Dispersion agent (A) is a pyrrolidone; Dispersion agent (B) is a special silica; Release agent is a light calcium carbonate; Initiator is a superoxide.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104250314A (en) * | 2014-02-25 | 2014-12-31 | 江苏煦和新材料有限公司 | Process for synthesis of high chlorinated medium viscosity metallocene polyethylene by aqueous phase suspension method |
| CN104311708A (en) * | 2014-10-30 | 2015-01-28 | 徐晨曦 | Method for preparing chloride metallocene polypropylene by acid-phase emulsion melting process |
| 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 |
| CN107141392A (en) * | 2017-06-30 | 2017-09-08 | 江苏中煦高分子材料有限公司 | A kind of chlorination linear low density polyethylene (LLDPE) synthesis technique |
| CN107365399A (en) * | 2017-06-30 | 2017-11-21 | 江苏中煦高分子材料有限公司 | A kind of chlorination linear low density polyethylene (LLDPE) |
| CN107868146A (en) * | 2017-12-08 | 2018-04-03 | 阳煤集团昔阳化工有限责任公司 | A kind of water phase suspension produces CPE new technologies |
| CN108912252A (en) * | 2018-06-12 | 2018-11-30 | 梁格 | A kind of In The Production Technology of Chlorinated Polyethylene |
| CN110606903A (en) * | 2019-08-23 | 2019-12-24 | 浙江晟祺实业有限公司 | Chlorinated linear low-density polyethylene and preparation method thereof |
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| CN101260168A (en) * | 2008-04-28 | 2008-09-10 | 江苏天腾化工有限公司 | Method for producing high-performance rubber type chlorinated polyethylene by water-phase method |
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2012
- 2012-06-14 CN CN2012101961172A patent/CN102690382A/en active Pending
Patent Citations (1)
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| CN101260168A (en) * | 2008-04-28 | 2008-09-10 | 江苏天腾化工有限公司 | Method for producing high-performance rubber type chlorinated polyethylene by water-phase method |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104250314A (en) * | 2014-02-25 | 2014-12-31 | 江苏煦和新材料有限公司 | Process for synthesis of high chlorinated medium viscosity metallocene polyethylene by aqueous phase suspension method |
| CN104250314B (en) * | 2014-02-25 | 2017-11-14 | 江苏煦和新材料有限公司 | Viscosity metallocene PE synthesis technique in the high chlorination of water phase suspension |
| CN104311708A (en) * | 2014-10-30 | 2015-01-28 | 徐晨曦 | Method for preparing chloride metallocene polypropylene by acid-phase emulsion melting process |
| CN104311708B (en) * | 2014-10-30 | 2016-08-17 | 徐晨曦 | A kind of method that acid phase emulsion fusion method prepares chlorination metallocene polypropylene |
| CN107141392A (en) * | 2017-06-30 | 2017-09-08 | 江苏中煦高分子材料有限公司 | A kind of chlorination linear low density polyethylene (LLDPE) synthesis technique |
| CN107365399A (en) * | 2017-06-30 | 2017-11-21 | 江苏中煦高分子材料有限公司 | A kind of chlorination linear low density polyethylene (LLDPE) |
| CN107141392B (en) * | 2017-06-30 | 2020-05-19 | 江苏中煦高分子材料有限公司 | Process for synthesizing chlorinated linear low-density polyethylene |
| CN107365399B (en) * | 2017-06-30 | 2020-05-19 | 江苏中煦高分子材料有限公司 | Chlorinated linear low-density polyethylene |
| CN107868146A (en) * | 2017-12-08 | 2018-04-03 | 阳煤集团昔阳化工有限责任公司 | A kind of water phase suspension produces CPE new technologies |
| CN108912252A (en) * | 2018-06-12 | 2018-11-30 | 梁格 | A kind of In The Production Technology of Chlorinated Polyethylene |
| CN110606903A (en) * | 2019-08-23 | 2019-12-24 | 浙江晟祺实业有限公司 | Chlorinated linear low-density polyethylene and preparation method thereof |
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Application publication date: 20120926 |