Method of producing base oil having low content of sulphur and ecologically clean aromatic filler materials and caoutchouc and rubber plasticisers

FIELD: chemistry.

SUBSTANCE: invention relates to a method of producing base oil with low content of sulphur, ecologically clean aromatic filler materials and caoutchouc and rubber plasticisers, involving selective purification of petroleum oil fractions with a selective solvent, separation of the first step extract and raffinate solutions, wherein the first step extract solution is cooled with subsequent separation a first step pseudo-raffinate solution in the settling tank, and after solvent regeneration, the first step raffinate solution is dewaxed and oxidised with subsequent extraction of the oxidised dewaxed oil to obtain second step raffinate and extract solutions; after solvent regeneration and subsequent adsorption or hydrofining, group II base oil with low sulphur content is obtained from the second step raffinate solution, wherein the second step extract solution is mixed with the first step pseudo-raffinate solution to obtain, after solvent regeneration, ecologically clean aromatic filler and a caoutchouc and rubber plasticiser with less than 2.9% content of polyaromatic hydrocarbons (PAH).

EFFECT: obtaining base oil with negligible sulphur content.

3 cl, 3 tbl, 3 dwg

 

The invention relates to the field of chemical technology and can be used in oil refining, in particular to obtain base oils group II (API) with a sulfur content of 0.03% and environmentally safe oil fillers and plasticizers with the content of polyaromatic hydrocarbons (PAH) less 2,9% (IP 346), used in the manufacture of rubber.

A prototype of the proposed method is a method for base oils, fillers and plasticizers for rubber according to the classic technology of oil production [1]. There are also different ways of getting fillers and plasticizers [2, 3]. As close analogues to the technical nature and essential features of the proposed method for producing base oils, fillers and plasticizers for rubber, it is possible to allocate the following ways:

Based on the procedure of oxidation of the oil distillate with hydrogen peroxide in the presence of catalyst, solvent extraction, dewaxing the raffinate and the receiving base oil with low sulfur content [2];

- Based on two-stage extraction separation of oil distillate, in which the first stage extraction (extractor) selective solvent interacts with the raw materials to receipt of the raffinate and extract solutions first article is fine and the subsequent regeneration of the solvent from these solutions to produce a raffinate and extract the first stage, which on second stage extraction interacts with the new portion of the selective solvent to obtain the raffinate and extract solutions of the second stage and the subsequent regeneration of the solvent from these solutions to produce a raffinate and extract the second stage [3].

According to sources [1, 2, 3] get the base oil is made according to the classical scheme of a single-stage treatment, which includes the vacuum distillation of fuel oil selective treatment of distillates, the dewaxing refined, Hydrotreating or adsorptive purification of dewaxed oils with obtaining the target product base oil, and a by-product of the extract of the first stage, which according to the method of [3] is subjected to separation in the second stage extraction with getting the raffinate and extract the second stage, the first of which is a filler and a plasticizer for rubber. The main disadvantage of classical technologies for base oils [1] is the inability to obtain a base oil group II with a sulfur content of 0.03%. The main disadvantage of this method [2] is the need to use fresh solvent in each stage of extraction, which leads to high total ratio of solvent on shared raw materials, availability of four blocks regeneration of the solvent and the high Lod is determined as being energy, that increases the cost of production. In addition, the second stage of extraction is characterized by a poor separability raffinate and extract solutions due to small differences in the densities of interactive products, which is confirmed by numerous laboratory experiments with purification of the extract with N-organic.

The invention consists in that in the production of oils classic set of processes is complemented stages: sludge extract solution to a temperature 5÷45°C depending on the PAH concentration in the raw material. If the content of PAH<7% the temperature of the sludge phase is carried out at a temperature of +5°C and below. The separated phase pseudorapidities solution is directed to the mixing with the extract solution selective treatment dewaxed oil, and then on the regeneration of the solvent with the receipt of filler and plasticizer for rubber containing less than 2.9% of PAH; stage oxidation dewaxed oil and its extraction with obtaining a base oil with a sulfur content of 0.05-0.08%. Adsorption or Hydrotreating allows you to bring the sulfur content in the base oil to 0.03%.

The main purpose of the present invention to provide a base oil group II with a sulfur content of 0.03%, as well as organic filler and plasticizer with the content is of PAHs less than 2.9 percent. This improves the technical-economic indicators, such as increasing selection of target products, the reduction ratio of solvent to raw material extraction, reducing energy costs for obtaining modern base oils, fillers and plasticizers for rubber. This goal is achieved by selective purification oil distillate and a vacuum residue, sludge at low temperatures the extract solution, the Department pseudorapidities solution with low content of PAHs, dewaxing the raffinate by its oxidation by hydrogen peroxide and other oxidants in the presence of a catalyst, single-stage extraction of oxidized dewaxed oil with getting the raffinate of the second step with a sulfur content of 0.05-0.08%, and the extract solution, which is mixed with pseudorapidity solution of the first stage of extraction, regeneration of the solvent with the receipt of filler and plasticizer with the PAH content of less than 2.9 percent. Adsorption or Hydrotreating the raffinate second stage sulfur content in it is brought up to 0.03%.

Addition to the classical technology of oils stage sludge extract solution of the first stage allows you to extract valuable components of the extract solution in the form pseudorapidities solution to 15%, which is mixed with extra who tym solution obtained by extraction of oxidized dewaxed oil. After regeneration of these solvent is obtained organic filler and plasticizer with the PAH content of less than 2.9 percent. Mixing pseudorapidities solution with the extract solution from the oxidized dewaxed oil allows you to boot the recovery system (optional) solvent (15% pseudorapidities solution and 25% of the extract solution from the oxidized dewaxed oil). Dewaxed oil is oxidized by hydrogen peroxide or other oxidizing agent in the presence of a catalyst acetone, oils, metals, etc. at a temperature of 20-80°C. the Oxidation of dewaxed oil allows you to turn the sulfide sulfur in the more polar sulfoxidov that fully extracts the solvent from the dewaxed oil (sulfur content reduced it to 4 or more times). Adsorption or Hydrotreating the raffinate oxidized dewaxed oil allow to obtain a base oil group II with a sulfur content of 0.03%.

As the selective solvent can be any selective solvent such as phenol, furfural, N-organic and others.

The set of distinctive features, described above, provides technical advantages of the proposed method: the expansion of the selection of environmentally friendly oil plasticizer and filler, obtaining a base oil group II due to the implementation of:

processes Department pseudorapidities solution sludge at low temperatures;

- oxidation and extraction of the dewaxed oil; adsorption and Hydrotreating the raffinate second stage;

- mixing pseudorapidities solution with the extract solution obtained by the extraction of oxidized dewaxed oil regeneration of these solvent to produce clean filler and plasticizer for rubber.

Figure 1 presents the scheme of separation of raw materials by a known method is a two - step scheme of separation of raw materials purification by selective solvent in the extractor first step to obtaining the raffinate and extract solutions and their regeneration (Department of solvent) to obtain a raffinate and extract, which is then separated in the extractor of the second stage of obtaining the extract solution of the second stage. After regeneration of the solvent is obtained extract, and after regeneration of the solvent from ravintola solution of the second stage is obtained filler and plasticizer for rubber with the PAH content of less than 2.9%.

Figure 2 presents the scheme of obtaining oil with low sulfur content. Oil distillate, vacuum residue is oxidized in the pipeline, separation of raw materials in Rafina is hydrated and the extract solution is held in the extractor first stage, after regeneration of the solvent is obtained raffinate with low sulphur content and extract oil plasticizer.

Figure 3 shows the proposed scheme for base oil group II with a sulfur content of 0.03%, as well as organic filler and plasticizer for rubber with the PAH content of less than 2.9 percent.

The figures below: 1 - extractor first stage; 2 - block the regeneration of the solvent from ravintola solution; 3 - block the regeneration of the solvent from the extract solution; 4 - extractor second stage; 5 - block regeneration of the solvent from ravintola solution from the second stage of extraction of the extract of the first stage; 6 - block regeneration of the solvent from the extract solution from the second stage of extraction of the extract of the first stage; 7 - dewaxing unit; 8 - sump, Department pseudorapidities solution; 9 - block regeneration of the solvent from the mixture pseudorapidities and the extract solution of the second stage; 10 - block regeneration of the solvent from the extract solution of the second speed; 11 - node oxidation; 12 - block regeneration of the solvent from ravintola solution of the second step; a 13 - block adsorption purification; 14 - condensers; I - raw materials; II - oxidant; III - solvent; IV - refined oils with low sulfur content; V - extract; VI - the raffinate of the first stage; VII - extract the first stage; VIII - ex is ract second stage; IX - raffinate second stage, filler and plasticizer for rubber (PAH less than 2.9%); X - refinity solution of the second stage; XI - dewaxed oil with low sulphur content; XII - base oil group II; XIII - filler and plasticizer for rubber with the PAH content of less than 2.9%.

Raw oil distillate, vacuum residue in the extractor first stage is mixed with the solvent and is output as the raffinate and extract solutions, after regeneration of the solvent from ravintola solution is obtained raffinate and the extract solution is cooled with getting pseudorapidities solution that is directed to the mixing with the extract solution obtained after extraction of the oxidized dewaxed oil. After regeneration of these solvent obtained oil plasticizer and a filler for rubber. And the raffinate after the first stage extraction deparaffinized, is oxidized by hydrogen peroxide or other oxidizing agent in the presence of a catalyst acetone, oils, metals, etc. at a temperature of 20-80°C and subjected to extraction in the extractor of the second stage, from which are derived the raffinate and extract solutions of the second stage. From ravintola solution of the second step is to regenerate the solvent. Refined oils with low sulfur content after the adsorption treatment or is hydrooxide contain 0.03% sulfur.

Implementation of extraction equipment may be different, for example, extraction columns, mixer-settlers, the rotary disk extractors, etc. In table 1, 2 and 3 presents data confirming the achievement of objectives - indicators of the processes and the quality of the resulting base oil, organic filler and softener of rubber known and proposed methods and the results of the test oil plasticizer obtained by the proposed method in the rubber.

To test the efficiency of the proposed method to laboratory studies of selective treatment of industrial raw materials oil distillate V faction or the vacuum residue to obtain a raffinate of raffinate and extract the second stage extraction dewaxed oil. Conditions of carrying out the processes of extraction, dewaxing and adsorption meet the industrial parameters of the process. The atmospheric pressure. Selective clearing oil fraction - the ratio of solvent to raw materials of 1.7:1, the temperature at the first stage 55°C, at the second stage 60°C, and the third 65°C. the Oxidation damaka is carried out at temperatures of 20-80°C, when applying a 3% hydrogen peroxide to raw materials. Dewaxing - the ratio of solvent to raw 4:1. The temperature of the final cooling of raw materials minus 28°C. the Block adsorbs the Onna cleaning-aluminosilicate adsorbent babe, the ratio of the adsorbent to the raw material of 0.3:1, the temperature of 40-60°C. the Settling - time of the extract solution of the first stage in the sump is 30-60 minutes.

The analysis of the obtained base oil, filler and plasticizer for rubber was carried out on the certified equipment.

The results obtained (Tables 1, 2, 3) show that the proposed method allows to obtain the base oil group II and increase the selection of environmentally friendly filler and plasticizer for rubber.

Table 1
Name of indicators of quality base oilsAccording to the methodThe proposed method (vacuum residue)
1. The kinematic viscosity at 100°C, cSt19,2519,04
2. Sulfur content, %0,40,03
3. The content of saturated hydrocarbons, %<90%92%

Table 2
Name of indicators of the quality of the oil, a plasticizer,% outputAccording to the methodThe proposed method (vacuum residue)
1. Density, kg/m3at 20°C-0,967
2. The kinematic viscosity at 1000C, cSt19,820,2
3. The content of PCA by iP346 (DMSO), wt.%2,50,74
4. The content of α-benzo (a) pyrene, ppm-0,5
5. Output %90% of extract40%

Table 3
IndicesMO-6 29%Oil filler and plasticizer for rubber (experienced) 29%
The Mooney viscosity, the river. units5047
The tensile strength, kg/cm2 229223
227219
Elongation at break667655
607606
Residual elongation, %19,518,5
16,015,5
The vulcanization time, min6060
8080
Content, % wt.:
- SU-10,300,28
butter29,329,0
- free organic acidsto 4.984,8
organic acids0,020,00
- volatile0,040,09
Break options (rubber mixture according to THE 2294-0,08-73776139-2009), 60 min, 150°C, ±1 arc
- M1, N*m - Minimum torque corresponding to the minimum torque to break the curve is proportional to the viscoelastic properties of the rubber compound at the temperature of vulcanization, describes its stiffness.1,111,10
- Mn, N*m Maximum torque corresponding to the maximum value of the torque of the vulcanization curve, is proportional to the shear modulus of rubber during curing temperature, which characterizes the stiffness of the rubber at the end of the vulcanization process.3,903,89
- Tsmin - the start Time of vulcanization, determined by the increase of the minimum torque of 0.1 N*m when the amplitude of the 1oand 0.2 N*m when the amplitude of the 3oand 5o.of 5.45,3
- top, min - Optimal vulcanization time for which achieves optimum properties the vulcanizer, it may differ from the actual optimum time required to reach optimum properties25,430,0
- Ry, min-1- The rate of vulcanization, is proportional to the average slope of the rising branch of the vulcanization curve.5,004,04

Literature

1. Selective cleaning of oil/ raw materials Regrigeration, Pasalimani and others - M.: Oil and gas, 1998. - 208 S., str-144.

2. Patent No. 2243986 from 02.10.2003 "Method of cleaning oil fractions" (C10G 53/04, C10G 53/14), the authors Nigmatullin V.R., V. Sharipov, Nigmatullin I.R.

3. Patent No. 2313562 from 27.12.2007, (C10G 21/22, SC 11/00), the authors of the Passages NV and others

1. The way to obtain base oils with low sulfur, clean aroma of fillers and plasticizers for rubber, including selective clearing oil oil fractions by selective solvent, separating the extract and ravintola solutions of the first stage, wherein the extract solution of the first stage is cooled, followed by the separation in the settler pseudorapidities solution of the first stage, and refinity solution of the first stage after the regeneration of the solvent deparaffinized and oxidized with subsequent extraction of the Oka is certain dewaxed oil with getting the raffinate and extract solutions of the second stage, from ravintola solution of the second stage after the regeneration of the solvent and subsequent adsorption or Hydrotreating get the base oil group II with low sulfur content, while the extract solution of the second stage is mixed with pseudorapidity solution of the first stage to obtaining after regeneration of the solvent, organic aromatic filler and plasticizer for rubber content of polyaromatic hydrocarbons (PAH) less than 2.9 percent.

2. The method according to claim 1, characterized in that the extract solution of the first stage is cooled to a temperature 5-45°C.

3. The method according to claim 1, wherein the dewaxed oil is oxidized by hydrogen peroxide in the presence of a catalyst selected from the group of acetone, oil, metals, at a temperature of 20-80°C.



 

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3 cl, 3 tbl, 3 dwg

FIELD: oil and gas production.

SUBSTANCE: invention relates to stabilisation of gas-saturated oil. Proposed method comprises two-stage separation at 20-80°C with separation of gas at 1st separation stage at 0.11-0.16 MPa. It comprises also separation of degassed oil at 2nd separation stage at 0.01-0.06 MPa to obtain separated oil and gas. Separated gas is sucked off by degassing device, for example, ejector operated on associated gas from oil field separation stage. Here, extracted gas is mixed with 1st separation stage gas. Produced gas mix is cut in stable condensate and dry gas. Then, stable condensate is mixed with separated oil to feed stabilised oil and dry gas to consuming equipment.

EFFECT: higher yield of separator oil.

3 ex, 1 tbl

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