CN1331994C - Oil removing method of petroleum ointment - Google Patents
Oil removing method of petroleum ointment Download PDFInfo
- Publication number
- CN1331994C CN1331994C CNB2004100209259A CN200410020925A CN1331994C CN 1331994 C CN1331994 C CN 1331994C CN B2004100209259 A CNB2004100209259 A CN B2004100209259A CN 200410020925 A CN200410020925 A CN 200410020925A CN 1331994 C CN1331994 C CN 1331994C
- Authority
- CN
- China
- Prior art keywords
- solvent
- wax
- slack
- oiling
- accordance
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The present invention relates to a novel method for preparing wax products by deoiling wax paste. At certain temperature, deoiled raw materials are pre-diluted by deoiling solvents and directly ejected with the solvents. The oil wax is separated from raw materials in the processes of cold dilution, extraction and separation. The ejected pressure of the raw materials is from 0.5 to 3.0MPa, the solvent extraction time is from 5 to 50 min and the extraction temperature is from-15 to 25 DEG C. Compared with the prior art, the present invention has the advantages that the present invention improves the deoiling effect, reduces the oil content of the deoiling wax and shortens the extraction time. The present invention is especially suitable for deoiling heavy distillate wax paste to produce high melting wax and microcrystal wax.
Description
Technical field
The present invention relates to a kind of slack wax de-oiling and produce the method for dewaxed oil, especially produce the method for high melting-point wax and Microcrystalline Wax from reduce pressure heavy ends slack wax or residue slack wax.
Background technology
The method of producing petroleum wax with slack wax mainly contains sweating de-oiling technology, solvent deoiling technology.Sweating de-oiling technology is owing to the energy consumption height, and treatment capacity is little, and the production cycle is long, is eliminated gradually.Solvent deoiling technology is the sophisticated technology that industrial production petroleum wax generally adopts.Solvent mainly is methylethylketone-toluene (MEK-TOL), and solvent ratio is 3～6: 1, adopt multipoint dilution technology, and 10～25 ℃ of de-oiling temperature are filtered and are adopted vacuum-type drum filter.This technology is comparatively ripe, and process is continuous, is lower than 62 ℃ of raw materials, oily wax good separating effect, dewaxed oil oil-containing＜0.5% for handling fusing point.
US4451353 introduces 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, dewaxed oil oil-containing＜0.5%, yield 35%.This technology wax yield is low, and is not suitable for handling than last running.In order to improve the de-oiling effect, GB84772 proposes to adopt MIBK-MEK as the de-oiling solvent, MIBK: MEK=60: 40 (weight ratios), solvent ratio 3: 1, two sections de-oilings.This patent only is applicable to produces the paraffin wax product that fusing point is lower than 62 ℃.
Above-mentioned technology is unwell to handles high melting-point wax and Microcrystalline Wax raw material.Heavier because of the feedstock fraction of high melting-point wax and Microcrystalline Wax, crystallization is finer and closely woven, and plate crystal is promptly arranged, and needle crystal is arranged again, and it is very serious to stop up filter cloth during filtration, needs frequent ground temperature filter wash cloth, and the dewaxed oil yield is very low, and oily wax separating effect is bad, and filtration velocity is slower.
EP 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, cooling gradually in the extractive process imports vacuum-type drum filter at last and filters, thereby obtains wax product in tower.This technology has been omitted baroque double-pipe crystallizer, has reduced energy consumption, and filtration velocity is higher than solvent crystallization.But,, influenced the de-oiling effect so the raw material dispersion is even inadequately because raw material is sent in the cooling tower by transferpump.
It also is to adopt rare cold technology that CN1362496A proposes, but raw material be directly spray into rare cold-solvent in the extraction tower in, spray pressure 0.5～3.0MPa, the raw material that sprays into is come by the solvent homodisperse of high speed rotating rapidly at a high speed, forms uniform suspension.This suspension rare cold-extraction tower in the moving process, obtain cooling, extracting gradually.Cooling, extracting time are 10～60 minutes, and extraction temperature is 0～25 ℃.When the temperature of suspension reaches 10～25 ℃, import vacuum-type drum filter and filter, thereby obtain wax product.What this technology formed in solvent is solid little wax ball, solvent is gradually to wax ball internal diffusion in the extractive process, dissolving oil or low melt wax wherein, then, spread in the solvent outside ball by concentration difference dissolved oil or low melt wax, so obtain the lower dewaxed oil of oil-containing, need the long extracting time, as handle the residual oil slack wax of oil-containing 20w%, spray pressure 1.0～1.5MPa, extraction solvent MEK: TOL=50: 50, solvent ratio 5: 1, extracting time 40～50min, 20 ℃～25 ℃ of de-oiling temperature, dewaxed oil oil-containing 3.6w%～3.8w%.Though compare with EP 0104890 technology, the dispersion effect of raw material in solvent improves, and separating oil wax separating effect makes moderate progress, and the oil-containing of dewaxed oil is also higher.
Summary of the invention
At the deficiencies in the prior art, the present invention proposes the novel method that petroleum paraffin product is produced in a kind of slack wax de-oiling, further improves oily wax separating effect.
The present invention is in rare cold de-oiling technology, before raw material enters cooling tower, dilutes in advance with the de-oiling solvent, and then, solution directly sprays under certain pressure in the solvent when being cooled to be higher than cloud point, forms evenly small wax ball.The wax ball with solvent counter current contact, extracting, when reaching the de-oiling temperature, adopts conventional separation method in rare cold de-oiling tower, with wax ball and solution separating, obtain the lower dewaxed oil of oil-containing.
Detailed process may further comprise the steps:
(1) with the de-oiling solvent raw material slack wax is diluted in advance;
(2) mixture of slack wax and de-oiling solvent is cooled to and is higher than its cloud point;
(3) mixture that obtains of step (2) spray into rare cold-solvent in the extraction tower in;
(4) when wax grain when mobile temperature reaches 10～25 ℃ in solvent, import conventional tripping device and carry out wax grain and solution separating, the slack wax of telling solution is told remaining solvent through distillation and is obtained the dewaxed oil product.
The described raw material slack wax of above-mentioned steps (1) can be various heavy ends slack waxs, and as the residual oil slack wax, subtract four line slack waxs, subtract three-way slack wax and second line of distillation slack wax etc., the slack wax oil-containing is less than 30w%, preferably less than 20w%.The de-oiling solvent and rare cold-solvent in the extraction tower is a same type.The pre-diluting solvent weight ratio of solvent and slack wax is 0.1～1.0, and preferable pre-thinning ratio is 0.5～0.8, dilutes temperature in advance for being higher than 5 ℃～18 ℃ of slack wax fusing points.Pre-dilution can be heated to uniform temp with slack wax and solvent, mixes then, also can mix the back reheat and mix.
The mixture of slack wax described in the step (2) and de-oiling solvent is cooled to and is higher than 1～10 ℃ of its cloud point.
The pressure that the described raw material of above-mentioned steps (3) sprays in the solvent is 0.5～3MPa, and the solvent dispersion that the raw material of high speed ejection is stirred at a high speed rapidly comes, and forms uniform suspension.Solvent temperature-15 ℃～30 ℃, solvent and raw material weight are than 2～6: carries out reverse the contact with solvent in 1 the extraction tower, extracting time 5～50min is preferably 10～30min.The de-oiling solvent is generally C for being any The suitable solvent and mixture
3～C
6Ketone, aromatic solvent or the mixture of several solvents wherein.
Raw material sprays in the cold solvent in the cooling tower being higher than cloud point temperature after pre-dilution, and moment forms the small wax ball of solid, forms φ 0.5～0.8mm wax ball and is evenly distributed in the solvent.The mixing solutions of slack wax and pre-diluting solvent is when forming the solid wax ball, and solvent has little time to dissolve in the cold solvent, just is enclosed in the wax ball, so the wax ball is not a solid sphere, and contains solvent in the wax ball.The wax ball is in cooling, extractive process, external solvent has been dissolved oil in the wax ball or low melt wax and has been formed many ducts, then be contained in the Oil solvent that contains of slack wax inside, by the inside and outside concentration difference of wax ball, can in the wax ball, enter the external solvent rapidly along the duct, at this moment the wax ball has formed cavity, and external solvent is easy to diffuse in the wax ball, further the oil or the low melt wax of extracting wax ball inside.Reach predetermined de-oiling temperature, with wax ball and oil-containing separated from solvent.Raw material can improve slack wax de-oiling effect through pre-dilution, shortens the duration of contact of wax ball and solvent.
The inventive method through pre-dilution process, helps the de-oiling of wax ball with the slack wax raw material, reduces the oleaginousness in the dewaxed oil, improves the processing power of device.Adaptation to raw material is strong, especially for handling high melting-point wax and Microcrystalline Wax raw material its superiority is arranged more.
Embodiment
Below in conjunction with embodiment, specify the solution of the present invention and effect.
Testing used raw material is residual oil slack wax and the slack wax that subtracts three-way cut, its character such as table 1.
Table 1 slack wax Physical Property Analysis
| Project | The residual oil slack wax | Subtract three-way slack wax |
| Density (20 ℃) kg/m 3 | 875.9 | 817.6 |
| Color (D1500), number | 8.0 | ＞8.0 |
| (dripping) fusing point, ℃ | 64 | 49.6 |
| Oil-containing, m% | 18.20 | 18.59 |
Embodiment 1
The frivolous slack wax of 200g is heated to 70 ℃, dilutes in advance with the solvent of equality of temperature, solvent is MEK-TOK.Then, in the time of will being cooled to be higher than cloud point, spray in the solvent that highly stirs, the small wax ball that forms φ 0.5～0.8mm is uniformly distributed in the solvent, the wax ball rare cold-carry out the reverse extracting that contacts with solvent in the extraction tower, when temperature reaches 20 ℃, enter conventional filter method separation wax grain and solution and obtain dewaxed oil.Test conditions and the results are shown in Table 2.
Embodiment 2
According to the process of embodiment 1, only change operational condition, test-results sees Table 2.
Embodiment 3
According to the process of embodiment 1, change operational condition, solvent changes MIBK-MEK into, and test-results sees Table 2.
Embodiment 4
To subtract three-way slack wax is raw material, according to the degreasing process of 1 book of embodiment, and operational condition and test-results such as table 2.
Embodiment 5
To subtract three-way slack wax is raw material, changes operational condition, and the de-oiling effect sees Table 2.
Embodiment 6
To subtract three-way slack wax is raw material, changes operational condition, and solvent changes MIBK-MEK into, and test-results sees Table 2.
Table 2 embodiment operational condition and product wax character
| Embodiment | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| Material temperature, ℃ | 70 | 75 | 80 | 55 | 60 | 65 |
| Pre-thinning ratio | 0.8 | 0.5 | 0.8 | 0.3 | 0.6 | 0.5 |
| Be cooled to and be higher than cloud point, ℃ | 6 | 4 | 2 | 5 | 8 | 2 |
| Spray pressure, MPa | 1.5 | 2.5 | 1.0 | 1.0 | 0.6 | 0.6 |
| Solvent composition (weight ratio) | MEK∶TOL 50∶50 | MEK∶TOL 50∶50 | MIBK∶MEK 80∶20 | MEK∶TOL 65∶35 | MEK∶TOL 65∶35 | MIBK∶MEK 70∶30 |
| Solvent temperature, ℃ | -5 | 0 | 5 | -5 | -10 | 5 |
| The extraction solvent ratio | 4 | 5 | 3 | 3 | 3 | 2.5 |
| The flushing ratio | 1 | 1 | 1 | 1 | 1 | 1 |
| The total solvent ratio | 5 | 6 | 4 | 4 | 4 | 3.5 |
| The extracting time, min | 30 | 50 | 20 | 20 | 15 | 10 |
| Filtration temperature, ℃ | 20 | 15 | 25 | 10 | 10 | 15 |
| Filtration velocity, kg/hs -1 | 194 | 205 | 216 | 234 | 226 | 242 |
| The wax product oil-containing, w% | 1.21 | 1.07 | 1.34 | 0.67 | 0.84 | 1.03 |
| The wax product fusing point, ℃ | 80.4 | 82.6 | 79.9 | 64.8 | 64.1 | 63.9 |
Show that from the test-results of embodiment raw material of the present invention helps the separation of oily wax through pre-dilution process, the oleaginousness in the dewaxed oil is low.
Claims (9)
1, a kind of slack wax de-oiling method adopts rare cold de-oiling technology, it is characterized in that may further comprise the steps:
(1) with the de-oiling solvent raw material slack wax is diluted in advance, the pre-dilution weight ratio of solvent and slack wax is 0.1～1.0;
(2) mixture of slack wax and de-oiling solvent is cooled to and is higher than 1～10 ℃ of its cloud point;
(3) mixture that obtains of step (2) spray into rare cold-solvent in the extraction tower in, form the wax grain;
(4) when wax grain when mobile temperature reaches 10～25 ℃ in solvent, lead-in separation device carries out wax grain and solution separating, and the wax grain of telling solution is told remaining solvent through distillation and obtained the dewaxed oil product.
2, in accordance with the method for claim 1, it is characterized in that the described raw material slack wax of step (1) is selected from the residual oil slack wax, subtracts four line slack waxs, subtracts reduced pressure distillate slack waxs such as three-way slack wax and second line of distillation slack wax.
3, in accordance with the method for claim 1, it is characterized in that the described de-oiling solvent of step (1) and rare cold-solvent in the extraction tower is a same type.
4, in accordance with the method for claim 1, it is characterized in that the described pre-dilution weight ratio of step (1) is 0.5～0.8.
5, in accordance with the method for claim 1, it is characterized in that the described pre-dilution temperature of step (1) is for being higher than 5 ℃～18 ℃ of slack wax fusing points.
6, in accordance with the method for claim 1, it is characterized in that the pressure that the described raw material of step (3) sprays in the solvent is 0.5～3MPa.
7, in accordance with the method for claim 1, it is characterized in that step (3) described rare cold-extraction tower internal solvent temperature is-15 ℃～30 ℃, solvent is 2～6: 1 with the raw material weight ratio.
8, in accordance with the method for claim 1, it is characterized in that the solvent described in step (1) and (3) is C
3～C
6Ketone, aromatic solvent or the mixture of several solvents wherein.
9, in accordance with the method for claim 1, it is characterized in that the described extracting time of step (3) is 5～50min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100209259A CN1331994C (en) | 2004-07-06 | 2004-07-06 | Oil removing method of petroleum ointment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100209259A CN1331994C (en) | 2004-07-06 | 2004-07-06 | Oil removing method of petroleum ointment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1718690A CN1718690A (en) | 2006-01-11 |
| CN1331994C true CN1331994C (en) | 2007-08-15 |
Family
ID=35930638
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004100209259A Expired - Fee Related CN1331994C (en) | 2004-07-06 | 2004-07-06 | Oil removing method of petroleum ointment |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1331994C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100528191C (en) * | 2004-04-14 | 2009-08-19 | 复旦大学附属中山医院 | Chinese medicine preparation for treating diabetes complication and its preparing method |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN112625747B (en) * | 2019-09-24 | 2022-09-02 | 内蒙古伊泰煤基新材料研究院有限公司 | Solvent deoiling device and method |
| CN112625746B (en) * | 2019-09-24 | 2022-08-30 | 内蒙古伊泰煤基新材料研究院有限公司 | Device and method for preparing high-quality wax |
| CN115651701B (en) * | 2022-11-03 | 2024-08-27 | 国家能源集团宁夏煤业有限责任公司 | Deoiling method and device for Fischer-Tropsch wax |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4378287A (en) * | 1975-10-24 | 1983-03-29 | Numol Corporation | Wax product |
| CN1362496A (en) * | 2001-01-05 | 2002-08-07 | 中国石油化工股份有限公司 | Petroleum ointment deoiling process to prepare wax product |
-
2004
- 2004-07-06 CN CNB2004100209259A patent/CN1331994C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4378287A (en) * | 1975-10-24 | 1983-03-29 | Numol Corporation | Wax product |
| CN1362496A (en) * | 2001-01-05 | 2002-08-07 | 中国石油化工股份有限公司 | Petroleum ointment deoiling process to prepare wax product |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100528191C (en) * | 2004-04-14 | 2009-08-19 | 复旦大学附属中山医院 | Chinese medicine preparation for treating diabetes complication and its preparing method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1718690A (en) | 2006-01-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101531690B (en) | New technology for extracting tea saponin and tea seed oil from tea seeds by using water as solvent | |
| CN101302187B (en) | Production process of carbazol and anthracene | |
| JP2009519357A (en) | Preparation method of vegetable oil and fat, plant crude protein and plant fiber by water leaching method | |
| CN1331994C (en) | Oil removing method of petroleum ointment | |
| CN112574785A (en) | Deoiling method and application of Fischer-Tropsch synthetic wax | |
| CA3119367C (en) | Method for synchronously pressing oilseeds and refining oil in solid-phase | |
| CN103131025A (en) | Method for extracting gutta percha from eucommia ulmoides nutshell | |
| CN106752069B (en) | A method of improving capsanthin stability | |
| CN108085129B (en) | Preparation method of wood wax oil | |
| CN111019755A (en) | Flaxseed oil CO2Supercritical extraction separation method | |
| CN105754651B (en) | A kind of solvent for ketone-benzol dewaxing process dilutes and cold wash method | |
| CN111304662A (en) | Preparation method of tea seed cake cleaning agent | |
| CN102766525B (en) | Method for squeezing tea seed oil at normal temperature | |
| JP2022508666A (en) | Method for producing oryzanol from soap stock containing oryzanol | |
| CN100406425C (en) | Method for refining long-chain biatomic acid | |
| CN105567421B (en) | Degumming process for fragrant camellia seed oil | |
| CN109517615A (en) | The preparation method of oily recovery method and lube base oil in spent bleaching clay | |
| CN105968015A (en) | Device for extracting plasticizer from filter residues and extracting method using same | |
| CN111592930A (en) | Preparation method of idesia polycarpa crude oil | |
| CN111772009A (en) | Method for preparing instant black tea by using green tea dust | |
| CN1144865C (en) | Petroleum ointment deoiling process to prepare wax product | |
| CN110003999A (en) | A kind of camellia seed cleaning powder and its preparation process | |
| CN108822957A (en) | A kind of changeable polar solvent producing grain and oil and method | |
| CN115646061B (en) | Method for preparing filter aid from corn fiber residues | |
| CN109694747B (en) | Keto-benzene dewaxing process for low-wax-content raw material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20070815 Termination date: 20110706 |