CN102675661A - Method for preparing spherical polyethylene micro-powder wax by polyethylene byproduct-polyethylene wax - Google Patents
Method for preparing spherical polyethylene micro-powder wax by polyethylene byproduct-polyethylene wax Download PDFInfo
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- CN102675661A CN102675661A CN2012101544808A CN201210154480A CN102675661A CN 102675661 A CN102675661 A CN 102675661A CN 2012101544808 A CN2012101544808 A CN 2012101544808A CN 201210154480 A CN201210154480 A CN 201210154480A CN 102675661 A CN102675661 A CN 102675661A
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Abstract
The invention provides a method for preparing spherical polyethylene micro-powder wax by polyethylene byproduct-polyethylene wax, which comprises the steps of: dissolving the polyethylene wax byproduct generated in the production process of polyethylene into organic solvent, adding surface active agent, stirring, cooling and precipitating the polyethylene micro-powder wax from the solvent. The obtained product has the average grain diameter of 18-22mu m, the melting point increased to 90.7 DEG C from 76.4 DEG C and the yield of 95%. The method is simple in operation and low in cost; the obtained product can be used for coating, paint, ink and automotive beauty wax, so that the application field of the polyethylene wax is expanded, and the additional value of the product is increased; and the solvent recovered by reduced pressure distillation can be recycled.
Description
Technical field
The invention belongs to technical field of polymer materials, particularly relate to Vilaterm by product polyethylene wax prepares micro mist wax through liquid phase method method.
Background technology
At present, the sub product of polyethylene device is one of main source of PEW, and in polyethylene production start-stop car process, can produce a spot of oligopolymer is polyethylene wax, but because its purity is low, and MWD is wide, melt temperature is low, has seriously limited its application.Application to Vilaterm by product low-melting-point polyethylene wax; Only be with processing wax disk(-sc) after its processing of simply decolouring; As low side purposes such as the insulating compound of the lubricant of plastic working, electrical condenser, X-former winding and non-blushing thinners; Can not satisfy the requirement of Masterbatch and printing ink processing, so use range is narrow, price is low, value-added content of product is low with polyethylene wax
[1]The micronization polyethylene wax value that has a wide range of applications at aspects such as coating, printing ink and car detailing waxes.
The preparation polyethylene micropowder wax mainly contains three kinds of approach at present: the one, and with physical methods such as mechanical disintegration, spraying drying and freeze grindings, the polyethylene micropowder wax size distribution that this method is produced is wide, and energy consumption is big; The 2nd, directly regulate the polymerization preparation, this method complex process; The 3rd, utilize the effect of chemical reagent, make the polyethylene wax molecule that forms dispersion state grow up to the particulate of expectation size.
[2]Liquid phase method comparatively speaking, technology is simple, cost is low.
CN101108984A discloses a kind of chemical method and mechanical combination process of polyethylene wax micro mistization, though the polyethylene micropowder wax that can obtain being evenly distributed, this method complex process, cost of material is higher, complex operation step, energy consumption is big.
Summary of the invention
The present invention is intended to solve the deficiency of prior art, provides a kind of polyethylene wax that utilizes the Vilaterm by-product to prepare the method for spherical polyethylene micropowder wax.
Described method, its step and condition are following:
1), in having the device of whisking appliance, add fusing point and be 62.5-86.4 ℃ Vilaterm by product polyethylene wax and with the polyethylene wax mass ratio be that the solvent of 5:1 dissolves, solvent temperature 90-100 ℃, dissolution time 30min obtains stable liquid system;
2) be that the water phase surfactant mixture of 1%-10% joins in the liquid system, with concentration; Stir in 90-100 ℃ of constant temperature HS; Place ice bath to cool off system then, speed of cooling is 1-5 ℃/s, treat that system temperature is room temperature after; Separate through suction filtration, the solid micro-powder that obtains is the thick product of polyethylene micropowder wax;
3), with the thick product of polyethylene micropowder wax with ethanol agitator treating 5 times, carry out suction filtration, the pressed powder that obtains promptly gets polyethylene micropowder wax at 60 ℃ of following vacuum-drying 4-5h; Its melting range of the polyethylene micropowder wax that obtains is 86.2-90.7 ℃, and median size is 18-22 μ m;
4), the feed liquid behind the suction filtration is reclaimed solvent through underpressure distillation, pressure is-0.1Mpa, 60 ℃ of temperature, and recovered solvent can utilize again;
Described solvent is the mixture of YLENE, normal heptane or both arbitrary proportions;
Described tensio-active agent is that mass ratio is the sodium lauryl sulphate of 2:1-6:1 and the mixture of polyoxyethylene glycol, and its consumption is the 1-3% of polyethylene wax quality;
Described step 2) HS stirs, and stirring intensity is 900-1000rpm, and churning time is 8-10h.
The fusing point of the polyethylene micropowder wax product that obtains is matched the accurate melting point detector mensuration of X-6 that hundred AudioCodes skill ltds produce, intensification voltage 100v with Beijing;
Fig. 1 is the electron scanning micrograph of the polyethylene micropowder wax product shape characteristic that obtains, and the JSM-5500LV sem observation of producing with Japan is also taken.
Beneficial effect:The invention provides a kind of method for preparing Vilaterm by product polyethylene wax micro mist.Employing is dissolved in Vilaterm by product polyethylene wax in the organic solvent, under the condition that adds tensio-active agent, after HS stirs, with the ice bath method polyethylene micropowder wax is precipitated out from solvent.The product median size that obtains is 22 μ m, and fusing point is brought up to 90.7 ℃.This method is simple to operate, and cost is low; The product that obtains can be used for coating, paint, printing ink processing and car detailing wax, has widened the Application Areas of polyethylene wax, has improved value-added content of product, and economic worth improves a lot; Can utilize again through the underpressure distillation recovered solvent.
Description of drawings
Fig. 1 is the electron scanning micrograph of the polyethylene micropowder wax that obtains of the present invention.
Embodiment 11), in having the device of whisking appliance; Add fusing point and be 62.5-86.4 ℃ Vilaterm by product polyethylene wax (production of Jilin Petrochemical company) 10.0g and dissolve with the YLENE 50.0g of polyethylene wax mass ratio 5:1; 90 ℃ of solvent temperatures; Dissolution time 30min obtains stable liquid system;
2) be 3%, with concentration; Mass ratio is that the sodium lauryl sulphate of 2:1 and the aqueous solution of polyoxyethylene glycol join in the liquid system, stirs 8h, stirring velocity 900rpm in 90 ℃ of constant temperature HS; Then system is placed ice bath; After reducing to room temperature with the speed of 1 ℃/s, separate through suction filtration, the solid micro-powder that obtains is the thick product of polyethylene micropowder wax;
3), the thick product of polyethylene micropowder wax is carried out suction filtration 5 times with the ethanol agitator treating, the pressed powder that obtains obtains ethene micro mist wax 9.4g at 60 ℃ of following vacuum-drying 4h, and its melting range is 84.2-89.5 ℃, and median size is 17-24 μ m, and productive rate is 94%;
4), the feed liquid behind the suction filtration is reclaimed solvent through underpressure distillation, pressure is-0.1Mpa, 60 ℃ of temperature, and recovered solvent can utilize again;
Embodiment 2Solvent described in the step 1) is a normal heptane, and solvent temperature is 100 ℃; Step 2) mass ratio of sodium lauryl sulphate and polyoxyethylene glycol is 3:1 in; Remaining is identical with embodiment 1.The polyethylene micropowder wax 9.3g that obtains, its melting range are 85.4-89.1 ℃, and median size is 16-33 μ m, productive rate 93%,
Embodiment 3Solvent described in the step 1) is that mass ratio is the YLENE of 1:12.5 and the mixture of normal heptane, 100 ℃ of solvent temperatures; Step 2) mass ratio of sodium lauryl sulphate and polyoxyethylene glycol is 4:1 in
,Its concentration of aqueous solution is 5%; Speed of cooling in the step 3) is 1.5 ℃/s; Remaining is identical with embodiment 1.Obtain polyethylene micropowder wax 9.1g, its melting range is 84.9-88.7 ℃, median size 22-31 μ m, and productive rate 91%,
Embodiment 4Solvent temperature described in the step 1) is 100 ℃; Step 2) stirring velocity in is 1000 rpm, mixes time 10h; Speed of cooling in the step 3) is 1.2 ℃/s; Remaining is identical with embodiment 1.Obtain polyethylene micropowder wax 9.5g, its melting range is 86.2-90.7 ℃, median size 18-22 μ m, and productive rate 95%,
Embodiment 5Solvent described in the step 1) is that mass ratio is the toluene of 1:1 and the mixture of normal heptane; Step 2) mass ratio of sodium lauryl sulphate and polyoxyethylene glycol is 5:1 in, stirring velocity 950rpm, churning time 9h; Remaining is identical with embodiment 1.Obtain polyethylene micropowder wax 9.2g, its melting range is 83.4-89.1 ℃, median size 20-30 μ m, productive rate 92%.
Reference:
[1] " production of petroleum wax and deep processing ", Zheng Lihui, Sheng Kuilong etc., Chemical Industry Press, 2008.3.
[2] " polymeric microball material ", horse radiance, Su Zhiguo etc., Chemical Industry Press, 2005.6.
Claims (6)
1. a method for preparing Vilaterm by product polyethylene wax micro mist is characterized in that, its step and condition are following:
1), in having the device of whisking appliance, add fusing point and be 62.5-86.4 ℃ Vilaterm by product polyethylene wax and with the polyethylene wax mass ratio be that the solvent of 5:1 dissolves, solvent temperature 90-100 ℃, dissolution time 30min obtains stable liquid system;
2) be that the water phase surfactant mixture of 1%-10% joins in the liquid system, with concentration; Stir in 90-100 ℃ of constant temperature HS; Place ice bath to cool off system then, speed of cooling is 1-5 ℃/s, treat that system temperature is room temperature after; Separate through suction filtration, the solid micro-powder that obtains is the thick product of polyethylene micropowder wax;
3), with the thick product of polyethylene micropowder wax with ethanol agitator treating 5 times, carry out suction filtration, the pressed powder that obtains promptly gets polyethylene micropowder wax at 60 ℃ of following vacuum-drying 4-5h; Its melting range of the polyethylene micropowder wax that obtains is 86.2-90.7 ℃, and median size is 18-22 μ m;
4), the feed liquid behind the suction filtration is reclaimed solvent through underpressure distillation, pressure is-0.1Mpa, 60 ℃ of temperature, and recovered solvent can utilize again;
Described solvent is the mixture of YLENE, normal heptane or both arbitrary proportions;
Described tensio-active agent is that mass ratio is the sodium lauryl sulphate of 2:1-6:1 and the mixture of polyoxyethylene glycol, and its consumption is the 1-3% of polyethylene wax quality;
Described step 2) HS stirs, and stirring intensity is 900-1000rpm, and churning time is 8-10h.
2. a kind of method for preparing Vilaterm by product polyethylene wax micro mist as claimed in claim 1 is characterized in that its step and condition are following:
1), in having the device of whisking appliance; Add fusing point and be 62.5-86.4 ℃ Vilaterm by product polyethylene wax (production of Jilin Petrochemical company) 10.0g and dissolve with the YLENE 50.0g of polyethylene wax mass ratio 5:1; 90 ℃ of solvent temperatures; Dissolution time 30min obtains stable liquid system;
2) be 1%, with concentration; Mass ratio is that the sodium lauryl sulphate of 2:1 and the aqueous solution of polyoxyethylene glycol join in the liquid system, stirs 8h, stirring velocity 900rpm in 90 ℃ of constant temperature HS; Then system is placed ice bath; After reducing to room temperature with the speed of 1 ℃/s, separate through suction filtration, the solid micro-powder that obtains is the thick product of polyethylene micropowder wax;
3), the thick product of polyethylene micropowder wax is carried out suction filtration 5 times with the ethanol agitator treating, the pressed powder that obtains obtains ethene micro mist wax 9.4g at 60 ℃ of following vacuum-drying 4h, and its melting range is 84.2-89.5 ℃, and median size is 17-24 μ m, and productive rate is 94%;
4), the feed liquid behind the suction filtration is reclaimed solvent through underpressure distillation, pressure is-0.1Mpa, 60 ℃ of temperature, and recovered solvent can utilize again.
3. a kind of method for preparing Vilaterm by product polyethylene wax micro mist as claimed in claim 2 is characterized in that the solvent described in the step 1) is a normal heptane, and solvent temperature is 100 ℃; Step 2) mass ratio of sodium lauryl sulphate and polyoxyethylene glycol is 3:1 in; Remaining is identical with claim 2.
4. a kind of method for preparing Vilaterm by product polyethylene wax micro mist as claimed in claim 2 is characterized in that, the solvent described in the step 1) is that mass ratio is the YLENE of 1:12.5 and the mixture of normal heptane, 100 ℃ of solvent temperatures; Step 2) mass ratio of sodium lauryl sulphate and polyoxyethylene glycol is 4:1 in; Speed of cooling in the step 3) is 1.5 ℃/s; Remaining is identical with claim 2.
5. the described a kind of method for preparing Vilaterm by product polyethylene wax micro mist of claim 2 is characterized in that the solvent temperature described in the step 1) is 100 ℃; Step 2) stirring velocity in is 1000 rpm, mixes time 10h; Speed of cooling in the step 3) is 1.2 ℃/s; Remaining is identical with claim 2.
6. the described a kind of method for preparing Vilaterm by product polyethylene wax micro mist of claim 2 is characterized in that, the solvent described in the step 1) is that mass ratio is the toluene of 1:1 and the mixture of normal heptane; Step 2) mass ratio of sodium lauryl sulphate and polyoxyethylene glycol is 5:1 in, stirring velocity 950rpm, churning time 9h; Remaining is identical with claim 2.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106947328A (en) * | 2017-04-06 | 2017-07-14 | 广德瑞邦涂料有限公司 | A kind of dumb light cathode electrodip painting |
| CN109438731A (en) * | 2018-11-15 | 2019-03-08 | 青岛赛诺新材料有限公司 | A kind of micro mist wax automatic production process method |
| CN111044660A (en) * | 2019-12-31 | 2020-04-21 | 广东联塑科技实业有限公司 | Analysis method for components and content of lubricant in calcium-zinc stabilizer |
| CN113845671A (en) * | 2021-09-30 | 2021-12-28 | 江苏天问新材料科技有限公司 | Preparation method of spherical polyethylene wax |
| CN115260536A (en) * | 2021-11-18 | 2022-11-01 | 江苏天问新材料科技有限公司 | Preparation method of spherical polyethylene micro-powder wax |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102408609A (en) * | 2011-11-09 | 2012-04-11 | 长春工业大学 | Method for separating polyethylene byproduct polyethylene wax |
-
2012
- 2012-05-18 CN CN2012101544808A patent/CN102675661A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102408609A (en) * | 2011-11-09 | 2012-04-11 | 长春工业大学 | Method for separating polyethylene byproduct polyethylene wax |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106947328A (en) * | 2017-04-06 | 2017-07-14 | 广德瑞邦涂料有限公司 | A kind of dumb light cathode electrodip painting |
| CN109438731A (en) * | 2018-11-15 | 2019-03-08 | 青岛赛诺新材料有限公司 | A kind of micro mist wax automatic production process method |
| CN111044660A (en) * | 2019-12-31 | 2020-04-21 | 广东联塑科技实业有限公司 | Analysis method for components and content of lubricant in calcium-zinc stabilizer |
| CN113845671A (en) * | 2021-09-30 | 2021-12-28 | 江苏天问新材料科技有限公司 | Preparation method of spherical polyethylene wax |
| CN115260536A (en) * | 2021-11-18 | 2022-11-01 | 江苏天问新材料科技有限公司 | Preparation method of spherical polyethylene micro-powder wax |
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Application publication date: 20120919 |