CN1064701C - Method for refining petroleum wax by using compound adsorption agent - Google Patents
Method for refining petroleum wax by using compound adsorption agent Download PDFInfo
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- CN1064701C CN1064701C CN97100158A CN97100158A CN1064701C CN 1064701 C CN1064701 C CN 1064701C CN 97100158 A CN97100158 A CN 97100158A CN 97100158 A CN97100158 A CN 97100158A CN 1064701 C CN1064701 C CN 1064701C
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Abstract
The present invention relates to a method for refining petroleum wax by a composite absorbing agent, wherein the composite absorbing agent contains FCC waste catalyst and active white clay. When directly used without treatments, the dosage of the FCC waste catalyst accounts for 20 to 30 wt% of the total dosage; when used after chemical treatments, the dosage of the FCC waste catalyst accounts for 35 to 45 wt% of the total dosage. As indicated by implementation results, the method of the present invention has the advantages of technological practicability and convenient operation. Compared with a method for refining petroleum wax by using active white clay as an absorbing agent, the method of the present invention can reduce the wax content of a filter cake, can increase filtration speed, and has obvious economical and social benefits.
Description
The present invention relates to a kind of method of utilizing the compound adsorbent refined wax.More particularly, the present invention relates to the compound adsorbent formed by two kinds of sorbent materials.A kind of is atlapulgite, and another kind is the FCC spent catalyst.
The FCC spent catalyst derives from the plant catalytic cracking unit.In ordinary production, the activity need fresh makeup catalyst for the agent of holdout device inner equilibrium draws off poiser.This part poiser can not be re-used as cracking catalyst, is called as the FCC spent catalyst.Past, the methods of burying that adopt will be discarded more.The FCC spent catalyst is buried to become more difficult and expensive but the rules of current environmental protection strictness make.
Catalytic cracking is the important means of oil refining deep processing, so all there is this type of device nearly all refinery.These devices have also produced a large amount of FCC spent catalyst when creating huge economic benefit.Therefore, the comprehensive utilization of carrying out the FCC spent catalyst is very significant.For example, present European refinery provides three kinds of potential use (Rcdo1phe Schmitt.Oil ﹠amp in building material field; Gas J., 1991,89 (46): 101), as make pitch weighting agent, common brick and cement Additive.The U.S. has also developed the technology of demetalization recycle to the decaying catalyst that has deposited heavy metal, and set up pilot plant (Elin frank J., " Fluid Cracking CatalystDemetallization; " NPRA Annual Meeting, San Francisco, Calif., March 19-21,1989).But complex process, cost is higher.Though it is do a lot in this regard at present, general not enough and deep.
Given this, the object of the invention is to provide a kind of method of utilizing the compound adsorbent refined wax, promptly seeks a novel method of utilizing the FCC spent catalyst effectively.Promptly in the paraffin adsorption refining process, with the FCC spent catalyst as a kind of sorbent material and the compound use of atlapulgite, thereby the FCC spent catalyst is turned waste into wealth, and reach the purpose that reduces paraffin production cost and favourable production operation.
As everyone knows, scale wax contains the impurity of lower concentration, as unsaturated aromatic hydrocarbon and heteroatoms hydrocarbon derivative.These impurity mostly have polarity, they to color, the light stability of paraffin, smell flavor etc. and all can produce detrimentally affect.
Form and different paraffin purposes according to different raw materials, can adopt different process for purification.Usually, process for purification can be divided into chemical refining and physics refining (refining with adsorbents just).Physics is refining to be compared with chemistry is refining, does not produce etching problem, the problem that does not also exist acid sludge to handle.In the paraffin industrial production, physics is made with extra care and is still comparatively widely used Technology.Make the typical physics of technology refining (also being refining with adsorbents) of sorbent material refined wax with atlapulgite.
Atlapulgite is to be made by the natural clay modification.Mainly contain pure aluminium silicate, generally account for more than 70%.Its aprotic acid center is formed by Si-AL-O.Increased the protonic acid center again by the carclazyte after the sour modification, so they there is adsorption to the colloid in the paraffin, bituminous matter isopolarity impurity.The main purpose of atlapulgite refined wax is to remove colloid, the bituminous matter in the paraffin, improves colorimetric and light stability.
And for the FCC spent catalyst, analytical results shows that they have similarity with atlapulgite on chemical constitution.Mainly contain pure aluminium silicate, its content is also more than 70%W.Its aprotic acid center is also formed by Si-AL-O.But on physical structure, they and atlapulgite are different.As strength ratio carclazyte height, specific surface area generally is lower than carclazyte, orifice throat ratio carclazyte rule, and pore volume is slightly higher than carclazyte.Therefore, the FCC spent catalyst also should have adsorption to the polar impurity in the paraffin, but because of the difference adsorptive power of physical structure can be different.Given this, the present invention as compound adsorbent, has developed a kind of method of utilizing the compound adsorbent refined wax with FCC spent catalyst and atlapulgite.
Fig. 1 is a compound adsorbent refined wax process flow sheet of the present invention.
The invention will be further described below in conjunction with accompanying drawing:
The present invention is the refining raw material of paraffin with refinery's ketone benzene dewaxed oil and cold press sweating wax material.Its raw material main character is generally: Sai Shi colorimetric number-9-2; Light stability number＞6.
The compound adsorbent that the present invention adopts atlapulgite and FCC spent catalyst to form carries out paraffin adsorption refining.Wherein the FCC spent catalyst belongs to bifurcation type molecular sieve catalyst, as RHZ-200, LCS-7, RHZ-300 etc.
Compare with the method that adopts the single-activity carclazyte to make the sorbent material refined wax, characteristics of the present invention are to keep total sorbent material to account under the constant situation of the weight percent of raw material, directly use the FCC spent catalyst to make sorbent material, its consumption can reach the 20-30%W of total dose.If the FCC spent catalyst is carried out chemical treatment, its consumption can reach the 35-45%W of total dose.From point of practical use, can preferentially select for use the former to avoid chemically treated trouble.
The present invention in refining with adsorbents paraffin process, the adsorption temp 115-145 of employing ℃.
Technological process of the present invention is divided into following steps: compound adsorbent and the paraffin raw material thorough mixing that will be made up of atlapulgite and FCC spent catalyst at first, keep specified adsorption temp 115-145 ℃ and adsorption time 20-45 minute then, filter again, smart wax is separated with filter cake.
By above condition, resulting smart wax product can reach refining purpose, and its main quality index is: Sai Shi colorimetric number ≮ 17; Light stability number ≯ 6.
The about 10-20%W of gained filter cake waxy oil can reduce 1.5-3%W when making refining with adsorbents paraffin than list with atlapulgite.
Compare with only making sorbent material refined wax technology with atlapulgite, the present invention has following tangible advantage and significant effect.
1, the invention process is convenient, can reduce production costs, and tangible economic benefit and social benefit are arranged.
2, the FCC spent catalyst that adopts in the compound adsorbent of the present invention not only has refining effect, and helps the filter effect, thereby can improve filtration velocity.
3, wax content descends in the filter cake of compound adsorbent of the present invention.
4, the FCC spent catalyst can directly use as sorbent material, also can re-use after chemical treatment.
5, the present invention has adopted the FCC spent catalyst in compound adsorbent, and making it turns waste into wealth, and for new way has been opened up in the development and use of FCC spent catalyst, has also correspondingly solved environmental issue simultaneously.
The following examples are to further specify of the present invention, rather than the restriction scope of the invention.
Example 1:
Compound adsorbent of the present invention is made up of the FCC spent catalyst of 100%W atlapulgite and 0%W.That is,, at first make sorbent material with the single-activity carclazyte for later contrast.
The raw material that adopts is the raw material of No. 58 semi-refined waxs, forms its character by ketone benzene dewaxed oil and cold press sweating material: the Sai Shi colorimetric number is-1, and light stability number is 7, and oleaginousness is 0.89%W.
The consumption that atlapulgite is made sorbent material is the 3%W of paraffin raw material.
The product index of No. 58 semi-refined waxs requires: Sai Shi colorimetric number ≮ 17, and light stability number ≯ 6, penetration degree (1/10mm) ≯, smell flavor number ≯ 2, oleaginousness≤1.6%W, inorganic assorted and moisture content.
Concrete implementation step is as follows:
The 1000g paraffin raw material is joined in the 2L there-necked flask of depositing thermometer, agitator, funnel fully, be heated to 125 ℃ then under constantly stirring, add the 30g atlapulgite, account for the 3%W of raw material with oil bath.Keep adsorption temp constant, and keep adsorption time 25miu.Carry out vacuum filtration then, smart wax is separated with filter cake.
The quality of the smart wax product of gained: the Sai Shi colorimetric number is 18, and light stability number is 6, and smelling flavor number is 2, and fusing point is 58.3 ℃, and oleaginousness is 0.8%W, and penetration degree (1/10mm) is 12.0, inorganic assorted and moisture content.As seen, the smart wax of gained can reach the product quality indicator requirement of No. 58 semi-refined waxs.
Waxy oil is 20%W in the resulting filter cake.Smart wax yield is 99.4%.
Embodiment 2:
Compound adsorbent of the present invention is by the atlapulgite of 80%W and 20% FCC spent catalyst (RHZ-200: LCS-7=1: 1) form.
The paraffin raw material, other operational conditions and the implementation step that adopt are identical with embodiment 1.
The smart wax that obtains thus can reach the product quality indicator of No. 58 semi-refined waxs, its quality: the Sai Shi colorimetric number is 18, and light stability number is 5, smelling flavor number is 2, and fusing point is 58.3 ℃, and oleaginousness is 0.74%W, penetration degree (1/10mm) is 11, inclusion-free and moisture content.
Embodiment 3:
Compound adsorbent of the present invention is by the atlapulgite of 70%W and the FCC spent catalyst (RHZ-200:LCS-7=1: 1) form of 30%W.
The paraffin raw material, other operational conditions and the implementation step that adopt are identical with embodiment 1.
The smart wax that obtains thus can reach the product quality indicator of No. 58 semi-refined waxs.Its Sai Shi colorimetric number is 20, and light stability number is 3, and smelling flavor number is 1, and fusing point is 52.3 ℃, and oleaginousness is 0.74%W, and penetration degree (1/10mm) is 11.2, inclusion-free and moisture content.
Gained filter cake waxy oil is 17%W, and than embodiment 1 decline 3%W, smart wax yield is 99.49%W.
But during the component of noting directly using the FCC spent catalyst to make compound sorbent material, its content can not be too high.When being increased to 40%W as its content, by above the same terms and step, the smart wax Sai Shi colorimetric that obtains number is 16, does not reach the quality product requirement of No. 58 semi-refined waxs.
Embodiment 4:
Compound adsorbent of the present invention is by the atlapulgite of 60%W and the modification FCC spent catalyst (RHZ-200: LCS-7=1: 1) form of 40%W.Modification FCC spent catalyst is through rare HNO
3The solution exchange, roasting makes again.
Press embodiment 1 identical raw material, other operational conditions and implementation step, can reach the smart wax of No. 58 semi-refined wax product quality indicators.Its quality: the Sai Shi colorimetric number is 19, and light stability number is 5, and smelling flavor number is 2, and fusing point is 58.4 ℃, and oleaginousness is 0.8%W, and penetration degree (1/10mm) is 11.8.
But when the content of modification FCC spent catalyst in compound adsorbent was increased to 50%W, its smart wax amount did not reach the salable product requirement, so modification FCC spent catalyst consumption can not be too high.
Embodiment 5:
According to embodiment 2,3, carry out commerical test first in March, 96 in our factory one system wax workshop.There is the clay-filtered paraffin device of two covers in this workshop.Every covering device year, processing power was about 3 tons/year.
In order to contrast, a cover is still only made sorbent material with atlapulgite, also promptly adopts the atlapulgite of 100%W and the FCC spent catalyst of 0%W, and its operational condition is undertaken by former scheme.1) and the atlapulgite of 74%W another set of employing compound adsorbent of the present invention wherein contains the FCC spent catalyst (RHZ-200: LCS-7=1: of the 26%W of direct use.Its refined wax technology is that continuous adsorption is refining, sees Fig. 1.
The raw material that adopts is No. 58 semi-refined wax material.Its character: fusing point is 58.2-60 ℃, and oil-containing is 0.88-1.38%W, and the Sai Shi colorimetric number is-9-2.
(1) only makes sorbent material with atlapulgite
The total add-on of former scheme sorbent material is the 3%W of raw material.
The adsorption temp of former scheme is 140 ℃.
The adsorption time of former scheme is 25-30min.
Press Fig. 1, products obtained therefrom can reach the qualified product quality of No. 58 semi-refined waxs.Its product property: the Sai Shi colorimetric number is 17-26, and light stability number is 4-6, and smelling flavor number is 2, penetration degree (1/10mm) 12.3-13.8, and oil-containing is 0.56-1.38%W, fusing point is 58.2-60 ℃, inorganic assorted and moisture content.The filter cake content of wax is 17%W.
(2) adopt recombiner of the present invention to make sorbent material
The total consumption of compound absorption of the present invention is the 3%W of raw material, is consistent with former scheme.
Adsorption temp of the present invention is 125 ℃.
The refining with adsorbents time of the present invention is 25-30min.
Press Fig. 1, resultant paraffin wax product can reach semi-refined wax qualified product quality No. 58.Its quality: the Sai Shi colorimetric number is 17-26, and light stability number is 4-6, smells flavor and number is 1-2, and fusing point is 58.2-60 ℃, inorganic assorted and moisture content.The filter cake content of wax is 15.29%W, and the filter cake content of wax when only making sorbent material with atlapulgite has reduced 1.7%W.
In addition from operating aspect, adopt multiple sorbent material of the present invention after, the raw material preheating temperature among Fig. 1 can descend 15 ℃, the liquid level of vacuum filter illustrates that than former scheme decline 30-40cm the FCC spent catalyst helps the filter effect.This can reduce because of raw material is heavy, the high vacuum filter overflow phenomena that causes of viscosity.FCC spent catalyst granularity is big in addition, intensity is high, makes filter cake texture loose, is easily struck off.These all help operation.This shows that enforcement of the present invention has tangible economic benefit and social benefit.
Claims (5)
1. method of utilizing the compound adsorbent refined wax, it is characterized in that: compound adsorbent is made up of atlapulgite and FCC spent catalyst, and when FCC spent catalyst during not by chemical treatment, its consumption is the 20-30% (w) of total dose; When FCC spent catalyst during by chemical treatment, its consumption is the 35-45% (w) of total dose, with compound adsorbent and paraffin raw material thorough mixing, keep specified adsorption temp 115-145 ℃ then, adsorption time 20-45 minute, filter at last, smart wax is separated with filter cake.
2. according to the described method of claim, it is characterized in that: described chemical treatment is to use rare HNO
3The FCC spent catalyst is carried out ion-exchange, and then roasting.
3. method according to claim 1 is characterized in that: described FCC spent catalyst is selected from Y zeolite catalyzer, RHZ-200, LCS-7, RHZ-300.
4. method according to claim 1 is characterized in that: described FCC spent catalyst can directly use, and also can use through after the chemical treatment.
5. method according to claim 1 is characterized in that: described refining with adsorbents can periodical operation, also can be operate continuously.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97100158A CN1064701C (en) | 1997-01-13 | 1997-01-13 | Method for refining petroleum wax by using compound adsorption agent |
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| CN97100158A CN1064701C (en) | 1997-01-13 | 1997-01-13 | Method for refining petroleum wax by using compound adsorption agent |
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| CN1161367A CN1161367A (en) | 1997-10-08 |
| CN1064701C true CN1064701C (en) | 2001-04-18 |
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| CN97100158A Expired - Fee Related CN1064701C (en) | 1997-01-13 | 1997-01-13 | Method for refining petroleum wax by using compound adsorption agent |
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| CN105148827A (en) * | 2015-10-13 | 2015-12-16 | 中国石油化工股份有限公司 | Method for preparing absorbing agent for chemical leakage accident by adopting waste catalytic cracking catalyst |
| CN112852481B (en) * | 2020-12-30 | 2022-12-27 | 国家能源集团宁夏煤业有限责任公司 | Method for decolorizing Fischer-Tropsch wax |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU819152A1 (en) * | 1978-06-21 | 1981-04-07 | Предприятие П/Я Р-6518 | Method of neutralizing paraffins |
| JPS62185786A (en) * | 1986-02-12 | 1987-08-14 | Nippon Mining Co Ltd | Manufacture of normal paraffin |
| CN1010954B (en) * | 1986-03-04 | 1990-12-26 | 保罗·伍尔曼公司 | Installtion for charging shaft furnace |
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1997
- 1997-01-13 CN CN97100158A patent/CN1064701C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU819152A1 (en) * | 1978-06-21 | 1981-04-07 | Предприятие П/Я Р-6518 | Method of neutralizing paraffins |
| JPS62185786A (en) * | 1986-02-12 | 1987-08-14 | Nippon Mining Co Ltd | Manufacture of normal paraffin |
| CN1010954B (en) * | 1986-03-04 | 1990-12-26 | 保罗·伍尔曼公司 | Installtion for charging shaft furnace |
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| CN1161367A (en) | 1997-10-08 |
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