CN1362496A - Petroleum ointment deoiling process to prepare wax product - Google Patents
Petroleum ointment deoiling process to prepare wax product Download PDFInfo
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- CN1362496A CN1362496A CN 01106047 CN01106047A CN1362496A CN 1362496 A CN1362496 A CN 1362496A CN 01106047 CN01106047 CN 01106047 CN 01106047 A CN01106047 A CN 01106047A CN 1362496 A CN1362496 A CN 1362496A
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Abstract
The method for preparing wax product with low oil content by means of petrolatum dewaxing process adopts a combined process including the steps of directly-jetting raw material in the solvent, diluting and woling, extracting and filtering, in which its jetting pressure is 0.5-3.0 MPa, extracting time is 10-60 min. and extracting temp. is 0-25 deg.C. Said invention features small solvent ratio, low energy consumption, low oil content is wax product and continuous technological process.
Description
The present invention relates to a kind of slack wax de-oiling and produce the method for wax product, particularly from slack wax, produce the method for high melting-point wax and Microcrystalline Wax.
Paraffin, especially high melting-point wax are important chemical material.Can be widely used for fields such as rubber, plastics, fine chemistry industry, daily-use chemical industry.The production method of paraffin mainly contains press for extracting juice wax-sweating process, solvent dewaxing and de-oiling technology, urea dewaxing process, dewaxing by molecular sieve technology and spray deoiling technology.
Press wax-sweating process owing to the energy consumption height, treatment capacity is little, seldom adopts.Urea dewaxing process, dewaxing by molecular sieve technology generally are to be used for handling the lighter raw material of fraction, produce whiteruss.
Solvent dewaxing and de-oiling technology is the maturation process that industrial production paraffin and lubricating oil generally adopt.Solvent is methylethylketone-toluene (MEK-TOL) or methyl iso-butyl ketone (MIBK)-methylethylketone (MIBK-MEK), solvent ratio 3～6: 1, adopt multipoint dilution technology, and dewaxing temperature-10～-25 ℃, 10～25 ℃ of de-oiling temperature are filtered and are adopted vacuum-type drum filter.This technology is comparatively ripe, and process is continuous, oily wax good separating effect, the wax product that is obtained, its oil-containing＜0.5%.
United States Patent (USP) 4451353 is introduced the method that paraffin wax product is produced in a kind of slack wax solvent deoiling.The de-oiling solvent is MEK-TOL, solvent ratio 3.5: 1,15 ℃ of filtration temperatures, two sections de-oilings, gained wax product oil-containing＜0.5%, yield 35%.But this technology wax yield is low, and is not suitable for handling the heavier raw material of cut.In order to improve the de-oiling effect, English Patent 84772 proposes to adopt MIBK-MEK to replace MEK-TOL, MIBK: MEK=60: 40 (volume ratios), solvent ratio 3: 1, two sections de-oilings as the de-oiling solvent.But only being applicable to, this patented technology produces the paraffin wax product that fusing point is lower than 62 ℃.USSR (Union of Soviet Socialist Republics) patent 1097647 has been described and added flocculating aids in degreasing process, improves filtration velocity.The flocculating aids of recommending is the vitriol of copper or iron, the normal paraffin of carbonatoms 20～24 and some pour point depressant.Flocculating aids consumption 0.042～5% (to raw material).But this patented technology is unwell to produces Microcrystalline Wax and high melting-point wax.Because produce the raw material of ceresine and high melting-point wax, cut is heavier, and crystallization is finer and closely woven, existing plate crystal, needle crystal is arranged again, and during filtration, it is very serious to stop up filter cloth, frequently ground temperature filter wash cloth, product wax yield is very low, even add flocculating aids, filtration velocity is still very slow.
German Patent 247695 is introduced the method for a kind of spray deoiling explained hereafter paraffin wax product and Microcrystalline Wax product.(1～2.0MPa) atomizing becomes microspheroidal to this method under certain pressure with raw material, with ethylene dichloride or MEK-TOL is extraction solvent, solvent ratio 6～8: 1, and solvent fully contacts in extraction tower with spherical raw material, in extractive process, solvent dissolves the oil in the spherical raw material to greatest extent.At last, this mixture filters in vacuum-type drum filter.Thereby oil-wax is separated, 10～25 ℃ of filtration temperatures.This patented technology has been utilized the characteristics of spherical material good penetrability, and filtration velocity is very fast, can be used to handle the residual oil slack wax, produces Microcrystalline Wax and high melting-point wax.The weak point of this patented technology is, solvent ratio is big, the energy consumption height, and the production cost height, product wax oil-containing is higher.In addition, spherical raw material disperses inhomogeneous sometimes in solvent, and caking produces stifled tower phenomenon easily, thereby influences the carrying out of degreasing process.
European patent 0104890 proposes to adopt rare cold technology to carry out oily wax to separate, and its technological process is: raw material is sent in the cooling tower, and this cooling tower is equipped with whipping appts, and the de-oiling solvent in the tower is owing to high degree of agitation is rotated, thereby raw material is scatter rapidly.The formed mixture of raw material and solvent, progressively cooling in the extractive process imports vacuum-type drum filter at last and filters, thereby obtains wax product in tower.This patented technology has been omitted baroque double-pipe crystallizer, has reduced energy consumption, and filtration velocity is higher than solvent crystallization.But because raw material is sent in the cooling tower by transferpump, so the raw material dispersion is even inadequately, influenced the de-oiling effect, filtration velocity is lower than spray method.
The objective of the invention is in order to overcome the deficiency of above-mentioned paraffin or Microcrystalline Wax production technology, propose the particularly preparation method of high melting-point wax and Microcrystalline Wax of a kind of de-oiling efficient height, solvent ratio is low, energy consumption is low paraffin.
Main process of the present invention comprises:
1. be raw material with the slack wax, raw material is heated to above 5～30 ℃ at its zero pour.Feedstock property is:
(1) zero pour is 45～75 ℃, preferably 55～68 ℃.
(2) oil-containing＜30% (w), preferably＜20% (w).
(3) carbon residue＜1.0% (w).
2. the de-oiling solvent is sent into rare cold-extraction tower, solvent C
3～C
6Ketone and/or aromatic hydrocarbons, as acetone, methylethylketone, methyl iso-butyl ketone (MIBK), benzene, toluene or wherein several mixtures, solvent volume is than 3～7: 1, preferably 4～6: 1, solvent temperature-15～15 ℃.Rare cold-extraction tower top has a whipping appts, its agitator arm directly to stretch in the solvent in the cooling tower, starts whipping appts, makes the linear velocity of stirring wing end reach 100～300cm/s.
3. raw material is directly sprayed into rare cold-solvent in the extraction tower in, spray pressure 0.5～3.0MPa, the raw material of ejection is come by the solvent homodisperse of high speed rotating rapidly at a high speed.Form suspension very uniformly, this suspension rare cold-extraction tower in the moving process, obtain gradually cooling off, extracting.Cooling, extracting time are 10～60 minutes, and extraction temperature is 0～25 ℃.
4. when the temperature of suspension reaches 10～25 ℃, import vacuum-type drum filter and filter, oil-wax is separated.
Characteristics of the present invention are that raw material directly sprays in solvent, have guaranteed that raw material is uniformly dispersed in solvent, help the conveying and the filtration of material.Produce paraffin, particularly high melting-point wax and Microcrystalline Wax according to method of the present invention, compare with rare cold technology with spray deoiling technology, solvent ratio reduces, energy consumption reduces, and product wax oil length reduces, and has improved the de-oiling effect, improve treatment capacity, avoided the caking phenomenon of material.
The inventive method is suitable for the production of inspissated wax and Microcrystalline Wax most, also can be used for the production of low melt point paraffin.Further specify the solution of the present invention and effect below in conjunction with embodiment.
Embodiment 1
The raw material that the embodiment of the invention and comparative example adopt is the residual oil slack wax and subtracts three-way slack wax.Its character sees Table 1.
Table 1 raw material slack wax character
Get 200 parts of raw materials (residual oil slack wax), be heated to 70 ℃, it is sprayed in 800 parts of solvents, form a kind of uniform suspension, this suspension rare cold-extraction tower in slowly the cooling.When the temperature of suspension is reduced to 10 ℃, send into the filtration operation and filter.Thereby obtain wax product.Operational condition and product property see Table 2.
| Project | The residual oil slack wax | Subtract three-way slack wax |
| Zero pour/℃ | ????63.5 | ????58 |
| Oleaginousness/w% | ????20 | ????15 |
| Carbon residue/w% | ????0.7 | ????0.5 |
| Density/g.cm -3 | ????0.8850 | ????0.8350 |
| Viscosity (100 ℃)/cps | ????8.0 | ????7.8 |
Embodiment 2
According to the method for embodiment 1, just change operational condition, the character of products obtained therefrom wax sees Table the test number 2 in 2.
Comparing embodiment 3
200 parts of raw materials spray in spray tower, obtain spherical raw material, should spherical raw material and 800 parts of solvent, in mixing process, oil in the raw material and low melt wax are dissolved by the de-oiling solvent, when the temperature of mixture is reduced to 10 ℃, send into filtering system and filter, obtain wax product, its character sees Table the test number 3 in 2.
Comparing embodiment 4
200 parts of raw materials are sent into cooling tower by transferpump, 800 parts of solvents are housed in the tower, and raw material is disperseed by the solvent of high speed rotating in the tower, when the temperature of mixture in the tower is reduced to 10 ℃, send into filtering system and filter, resulting product wax character sees Table the test number 4 in 2.
Embodiment 5
According to embodiment 1 described method, change operational condition, solvent changes MEK-TOL into, and the product wax character of gained sees Table the test number 5 in 2.
Embodiment 6
According to embodiment 5 described methods, spray pressure changes 1.5MPa into, and operation index and product property see Table the test number 6 in 2.
Embodiment 7
To subtract three-way slack wax is raw material, and according to embodiment 1 described method, resulting wax product character sees Table the test number 7 in 2.
Comparing embodiment 8
According to comparing embodiment 3 described methods, raw material changes into and subtracts three-way slack wax, and operation index and product property see Table the test number 8 in 2.
Table 2 operational condition and product property
Continuous table 2
| Test number | ????1 | ????2 | 3 (comparative examples) | 4 (comparative examples) |
| Raw material | The residual oil slack wax | The residual oil slack wax | The residual oil slack wax | The residual oil slack wax |
| Material temperature/℃ | ????70 | ????80 | ????70 | ????70 |
| Spray pressure/MPa | ????0.6 | ????0.6 | ????0.6 | |
| Solvent composition (volume ratio) | MIBK∶MEK ＝50∶50 | ?MIBK∶MEK ?＝50∶50 | ?MIBK∶MEK ?＝50∶50 | ?MIBK∶MEK ?＝50∶50 |
| Solvent temperature/℃ | ????-5 | ????0 | ????-5 | |
| The solvent cut ratio | ????4 | ????5 | ????4 | ????4 |
| The flushing ratio | ????1 | ????1 | ????1 | ????1 |
| The total solvent ratio | ????5 | ????6 | ????5 | ????5 |
| Extracting time/min | ????15 | ????30 | ????15 | ????15 |
| Terminal linear velocity/the cm.s of stirring wing -1 | ????160 | ????200 | ????160 | |
| Filtration temperature/℃ | ????10 | ????15 | ????10 | ????10 |
| Filtration velocity/kg/h.m 2 | ????180 | ????183 | ????185 | ????135 |
| Product wax oil-containing/% | ????4.1 | ????3.7 | ????5.3 | ????5.1 |
| Melt drop temperature/℃ | ????67.2 | ????67.8 | ????66.0 | ????66.2 |
| Test number | ????5 | ????6 | ????7 | 8 (comparative examples) |
| Raw material | The residual oil slack wax | The residual oil slack wax | Subtract three-way slack wax | Subtract three-way slack wax |
| Material temperature/℃ | ????85 | ????80 | ???65 | ????70 |
| Spray pressure/MPa | ????1.0 | ????1.5 | ???0.8 | ????1.0 |
| Solvent composition (volume ratio) | ?MEK∶TOL＝ ??50∶50 | ?MEK∶TOL＝ ??50∶50 | MIBK∶MEK ＝50∶50 | MIBK∶MEK ＝50∶50 |
| Solvent temperature/℃ | ????5 | ????0 | ????-5 | |
| The solvent cut ratio | ????4 | ????4 | ????4 | ????4 |
| The flushing ratio | ????1 | ????1 | ????1 | ????1 |
| The total solvent ratio | ????5 | ????5 | ????5 | ????5 |
| Extracting time/min | ????40 | ????50 | ????20 | ????15 |
| Terminal linear velocity/the cm.s of stirring wing -1 | ????240 | ????260 | ????200 | |
| Filtration temperature/℃ | ????20 | ????25 | ????15 | ????10 |
| Filtration velocity/kg/h.m 2 | ????186 | ????190 | ????206 | ????210 |
| Product wax oil-containing/% | ????3.8 | ????3.6 | ????3.2 | ????4.7 |
| Melt drop temperature/℃ | ????67.8 | ????68.0 | ????69.0 | ????66.5 |
As can be seen from Table 2, adopt the technology of the present invention, promptly adopt spraying-rare cold combination de-oiling technology, produce high melting-point wax and Microcrystalline Wax, product wax oil-containing is low, contains oil index and meets national standard, and filtration velocity is faster than rare cold process, solvent ratio is little, has reduced energy consumption, has improved treatment capacity.
Claims (13)
1, a kind of is the method for raw material production wax with the slack wax, may further comprise the steps:
(1) slack wax is heated to above its zero pour;
(2) slack wax after will heating is with in the vaporific solvent that sprays into stirring;
(3) Wu Hua slack wax contacts also extracting with solvent, cooling forms suspension liquid;
(4) filter above-mentioned suspension liquid and obtain the dewaxed oil product.
2, in accordance with the method for claim 1, it is characterized in that described slack wax Heating temperature is for being higher than 5～30 ℃ at its zero pour.
3,, it is characterized in that the character of described slack wax is: 45～75 ℃ at zero pour, oil-containing＜30w% according to claim 1 or 2 described methods.
4, in accordance with the method for claim 3, it is characterized in that the character of described slack wax is: 55～68 ℃ at zero pour, oil-containing＜20w%.
5, in accordance with the method for claim 1, the spray pressure that it is characterized in that slack wax is 0.5～3.0MPa.
6, in accordance with the method for claim 1, the stirring intensity that it is characterized in that solvent is: the linear velocity 100～300cm/s at stirring wing tip.
7, in accordance with the method for claim 1, the temperature that it is characterized in that solvent is-15～15 ℃.
8, in accordance with the method for claim 1, it is characterized in that de-oiling solvent volume ratio is 3～7: 1.
9, in accordance with the method for claim 8, it is characterized in that de-oiling solvent volume ratio is 4～6: 1.
10, in accordance with the method for claim 1, it is characterized in that described solvent is selected from C
3～C
6Ketone and/or aromatic solvent.
11, in accordance with the method for claim 10, it is characterized in that described solvent is selected from acetone, methylethylketone, methyl iso-butyl ketone (MIBK), benzene, toluene or wherein several mixtures.
12, in accordance with the method for claim 1, it is characterized in that described extracting, cooling time are 10～60 minutes.
13, in accordance with the method for claim 1, it is characterized in that described filtration temperature is 10～25 ℃.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011060476A CN1144865C (en) | 2001-01-05 | 2001-01-05 | Petroleum ointment deoiling process to prepare wax product |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011060476A CN1144865C (en) | 2001-01-05 | 2001-01-05 | Petroleum ointment deoiling process to prepare wax product |
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| Publication Number | Publication Date |
|---|---|
| CN1362496A true CN1362496A (en) | 2002-08-07 |
| CN1144865C CN1144865C (en) | 2004-04-07 |
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|---|---|---|---|
| CNB011060476A Expired - Lifetime CN1144865C (en) | 2001-01-05 | 2001-01-05 | Petroleum ointment deoiling process to prepare wax product |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1331994C (en) * | 2004-07-06 | 2007-08-15 | 中国石油化工股份有限公司 | Oil removing method of petroleum ointment |
| CN109652125A (en) * | 2018-11-14 | 2019-04-19 | 山东源根石油化工有限公司 | A kind of OIL IN LUBRICATING OIL PRODUCTION clout recovery method |
-
2001
- 2001-01-05 CN CNB011060476A patent/CN1144865C/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1331994C (en) * | 2004-07-06 | 2007-08-15 | 中国石油化工股份有限公司 | Oil removing method of petroleum ointment |
| CN109652125A (en) * | 2018-11-14 | 2019-04-19 | 山东源根石油化工有限公司 | A kind of OIL IN LUBRICATING OIL PRODUCTION clout recovery method |
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| Publication number | Publication date |
|---|---|
| CN1144865C (en) | 2004-04-07 |
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Granted publication date: 20040407 |