CN1030282C - Method for removing impurities from olefine polymer and heavy oil - Google Patents
Method for removing impurities from olefine polymer and heavy oil Download PDFInfo
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- CN1030282C CN1030282C CN 90104731 CN90104731A CN1030282C CN 1030282 C CN1030282 C CN 1030282C CN 90104731 CN90104731 CN 90104731 CN 90104731 A CN90104731 A CN 90104731A CN 1030282 C CN1030282 C CN 1030282C
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Abstract
The present invention introduces a method for removing impurities from olefin polymers and heavy oil. The present invention is characterized in that solid or colloid impurities are separated from liquid through the interaction of a silicate gelling agent and impurities. The present invention has the advantages of easy operation, simple equipment requirement, easy acquirement of raw material, low price, good treating effect, etc.
Description
The present invention is the method that removes impurity from olefin polymer and mink cell focus.
In olefin polymer (as poly--alhpa olefin), used lubricating oil, steam cracking residual oil, catalytic pyrolysis residual oil, coal tar and shale oil, often contain a certain amount of impurity.This type of impurity is many to be existed with colloidal state, is difficult to remove with methods such as common sedimentation or filtrations.Japanese Patent J7418114; introduced a kind of method of pure esterification and pure esterification/washing under nitrogen protection among J7487783 and the J7732089; be used for removing the residual Ziegler/Natta catalyst of polypropylene slurry; reduced the ash in the product; but this method needs nitrogen protection in operating process; dewatering time is long, easily causes emulsification simultaneously in washing, brings difficulty to operation.USP4204946 has introduced among USP4420389 and the USP4705622 and has a kind ofly handled various mink cell focuses with the aqueous solution of ammonium salt or phosphonium salt under certain pressure, to remove the method for impurity; Introduced among the USP4539099 and a kind ofly handled oil product as jelling agent with alkoxyl group resol ethylene glycol fat, and then filtering method.But the former needs pressurized operation, and is higher to equipment requirements; As jelling agent, cost is higher with alkoxyl group resol ethylene glycol fat for the latter.
The objective of the invention is to overcome shortcoming of the prior art, provide a kind of and have easy and simple to handlely, equipment requirements is simple, and raw material is easy to get and the cheap method that removes impurity.
Technical characterictic of the present invention is the interaction by silicate gelling agent and impurity, makes solid or colloidal impurity and liquid separation, and concrete operations are as follows:
(1) adding 1～10m%(in the material that contains impurity is benchmark with the weight of material) silicate gelling agent, under 60～90 ℃, be stirred to and mix,
(2) adding 0.2～4.0m%(in above-mentioned mixed solution is benchmark with the weight of material) low molecular acid or low mass molecule alcohol condensing agent fully stir,
(3) impurity of separating out is removed with partition method or dissolution method.
Silicate gelling agent of the present invention is water glass or silicon sol; Described low molecular acid or low mass molecule alcohol condensing agent are acetic acid, oxalic acid, sulfuric acid or methyl alcohol, ethanol.It is benchmark with the weight of material that the consumption of silicate gelling agent is preferably 3～7m%(); It is benchmark with the weight of material that the consumption of low molecular acid or low mass molecule alcohol condensing agent is preferably 1～2m%().
The present invention compared with prior art adopts atmospheric operation, makes easy and simple to handlely, and equipment requirements is simple; The present invention has adopted raw materials such as silicate gelling agent, is easy to get and cheap; The present invention has excellent treatment effect, as with pure esterification/WATER-WASHING METHOD ratio, ash and impurity level all reduce significantly.
The present invention is applicable to from olefin polymer and/or lubricating oil, remove the process of impurity in steam cracking residual oil, catalytic pyrolysis residual oil, coal tar and the shale oil, be specially adapted to remove the process of remaining catalyst impurities from poly--alhpa olefin as the transformer oil pour point depressant.
Described gathering-alhpa olefin is a raw material with the soap wax olefin cracking normally, (is TiCl at Ziegler/Natta
3/ triisobutyl aluminium) polymerization under the effect of catalyzer, thus the mixing solutions of poly-alpha olefins and Ziegler/Natta catalyst obtained.
Further describe characteristics of the present invention below in conjunction with example.
Example 1
With molecular weight is 310,000 the poly-alpha olefins and the mixing solutions of catalyzer, place there-necked flask, adding 5m%(under nitrogen protection is benchmark with the weight of this mixed solution) concentration is the ethanol (Beijing Chemical Plant's production) of 95m%, be heated to 65 ℃, stir, make its esterification, generate water-soluble titanium and/or aluminic acid ester; After adding kerosene (weight with this mixed solution the is benchmark) dilution of 50m%, use tap water, washing is to neutral under 85 ℃ of stirrings.Be benchmark with 50m%(with the weight of this mixed solution again) 150SN turbine oil (production of Dalian oil seven factories) dilution, steam then and remove unreacted reactant and kerosene, obtain poly-alpha-olefin pour depressant, its impurity level and grey deal see Table 1.
Example 2
With molecular weight is 310,000 the poly-alpha olefins and the mixing solutions of catalyzer, places there-necked flask, add kerosene (weight with this mixed solution the is benchmark) dilution of 50m% after, in that to add 5m%(be benchmark with the weight of this mixed solution) contain SiO
2Concentration is the water glass (production of water glass plant, Tianjin) of 30m%, 65 ℃ were stirred 20 minutes down, adding 5m%(again is benchmark with the weight of this mixed solution) concentration is that the ethanol (Beijing Chemical Plant's production) of 95m% continues to stir 10 minutes, the centrifugal slag that takes off, be benchmark with 50m%(with the weight of this mixed solution again) 150SN turbine oil (production of Dalian oil seven factories) dilution, steam then and remove unreacted reactant and kerosene, obtain poly-alpha-olefin pour depressant, its impurity level and grey deal see Table 1.
Example 3
With molecular weight is 150,000 the poly-alpha olefins and the mixing solutions of catalyzer, places there-necked flask, and adding 7m%(is benchmark with the weight of this mixed solution) SiO
2Concentration is the water glass (production of water glass plant, Tianjin) of 30m%, 65 ℃ were stirred 20 minutes down, adding 2m%(again is benchmark with the weight of this mixed solution) concentration is that the ethanol (Beijing Chemical Plant's production) of 95m% continues to stir 10 minutes, add water, being heated to 85 ℃ left standstill 30 minutes, make the sodium silicate gel sedimentation and dissolve in the water, remove water layer; Add water again and repeat aforesaid operations.And then to add 50m%(be benchmark with the weight of this mixed solution) 150SN turbine oil (productions of Dalian oil seven factories) dilution, steam except that unreacted reactant and kerosene at last, obtain poly-alpha-olefin pour depressant, its grey deal is 375ppm.
Example 4
With molecular weight is 16.8 ten thousand the poly-alpha olefins and the mixing solutions of catalyzer, places there-necked flask, and adding 7m%(is benchmark with the weight of this mixed solution) SiO
2Concentration is the water glass (production of water glass plant, Tianjin) of 30m%, 70 ℃ were stirred 30 minutes down, adding 2m%(again is benchmark with the weight of this mixed solution) concentration is that the ethanol (Beijing Chemical Plant's production) of 95m% continues to stir 30 minutes, add water, be heated to 100 ℃ of dehydrations, adding 1m%(again is benchmark with the weight of this mixed solution) flocculating aids (Changbai county flocculating aids factory produces, trade mark CB-102H) filtered while hot, and then to add 50m%(be benchmark with the weight of this mixed solution) 150SN turbine oil (productions of Dalian oil seven factories) dilute, steam and remove unreacted reactant, obtain poly-alpha-olefin pour depressant, its grey deal is 120ppm.
Example 5
With molecular weight is 15.6 ten thousand the poly-alpha olefins and the mixing solutions of catalyzer, places there-necked flask, and adding 9m%(is benchmark with the weight of this mixed solution) silicon sol (chemical plant, Jiangyin produces, and contains 25m%SiO
2, 0.5m%Na
2O), be heated to 85 ℃, fully stirring the back, to add 2m%(be benchmark with the weight of this mixed solution) acetic acid (Beijing Chemical Plant's productions), continue stirring 60 minutes, be warming up to 110 ℃ of dehydrations; Adding 1m%(again is benchmark with the weight of this mixed solution) flocculating aids (Changbai county flocculating aids factory produces, trade mark CB-102H) filtered while hot, and then to add 50m%(be benchmark with the weight of this mixed solution) 150SN turbine oil (productions of Dalian oil seven factories) dilute, steam and remove unreacted reactant, obtain poly-alpha-olefin pour depressant, its grey deal is 205ppm.
Example 6
Get 500 gram used SAE40 diesel engine oils (being dark-brown, solid impurity content 869ppm), be placed in the there-necked flask, add 3.5 gram SiO
2Concentration is the water glass (production of water glass plant, Tianjin) of 30m%, stirs 30 minutes down at 75 ℃, adds 1 gram ethanol again, continues to stir 10 minutes, is warming up to 120 ℃ of dehydrations, again the elimination sodium silicate gel.The solids content of gained oil product is 190ppm.
Table 1
The ash content of coal metallic impurity amount (ppm) angle of loss *
Post-treating method
（ppm） Al Ti （%）
Esterification/WATER-WASHING METHOD 800 5.7 * 10
-45.3 * 10
-40.70
Soluble glass method 500 8.5 * 10
-59.1 * 10
-50.23
*: the poly-alpha olefins that obtains after referring to handle with above-mentioned two methods, join in the transformer oil of same amount with same amount respectively, according to ministerial standard SY2654-82, the angle of loss of the transformer oil that in the time of 70 ℃, records (the standard code angle of loss answers＜0.5).
Claims (6)
1, a kind of method that removes impurity from olefin polymer and mink cell focus comprises the process that adopts the jelling agent material handling, it is characterized in that adopting the interaction of a kind of silicate gelling agent and impurity, makes impurity and liquid separation, and the concrete operations step is as follows:
(1) in containing the material of impurity, add silicate gelling agent, its amount is 1～10m% of total inventory, mixes under 60～90 ℃;
(2) add in (1) step mixed solution and be selected from low molecular acid or the low mass molecule alcohol any as condensing agent, its amount be 0.2～4.0m% of total inventory, fully stirring;
(3) impurity of separating out is removed by separation or any method of dissolved.
2,, it is characterized in that described silicate gelling agent is water glass or silicon sol according to the described method that removes impurity of claim 1.
3,, it is characterized in that described low molecular acid condensing agent is acetic acid, oxalic acid or sulfuric acid according to the described method that removes impurity of claim 1.
4,, it is characterized in that described low mass molecule alcohol condensing agent is methyl alcohol or ethanol according to the described method that removes impurity of claim 1.
5, according to the described method that removes impurity of claim 1, the amount that it is characterized in that adding silicate gelling agent is 3～7m% of total inventory.
6, according to the described method that removes impurity of claim 1, the amount that it is characterized in that adding condensing agent is 1～2m% of total inventory.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90104731 CN1030282C (en) | 1990-07-23 | 1990-07-23 | Method for removing impurities from olefine polymer and heavy oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90104731 CN1030282C (en) | 1990-07-23 | 1990-07-23 | Method for removing impurities from olefine polymer and heavy oil |
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| Publication Number | Publication Date |
|---|---|
| CN1058351A CN1058351A (en) | 1992-02-05 |
| CN1030282C true CN1030282C (en) | 1995-11-22 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 90104731 Expired - Fee Related CN1030282C (en) | 1990-07-23 | 1990-07-23 | Method for removing impurities from olefine polymer and heavy oil |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1939935B (en) * | 2005-09-28 | 2010-04-14 | 中国石油化工股份有限公司 | Removal of catalyst impurities from olefine polymer |
| CN102977230B (en) * | 2011-09-05 | 2015-07-01 | 中国石油化工股份有限公司 | Method for removing hydrogenation catalyst in polymer solution |
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1990
- 1990-07-23 CN CN 90104731 patent/CN1030282C/en not_active Expired - Fee Related
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| CN1058351A (en) | 1992-02-05 |
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