CN100425677C - Processing method of softening oil (paraffin base) - Google Patents

Abstract

The invention relates the processing method for paraffinic base. It has good oxidation resistance and low volatility, and the butadiene rubber inner tube made by the paraffinic base has good oxidation resistance and long life. The method comprises the following steps: A making mother liquid: putting the paraffinic base into the still, heating to 65+-5Deg.C, stirring, then adding 2,6-ditrertiarybutyl p-methylphenyl; stirring with agitator and geared pump; B making product oil: putting the paraffinic base into finished product jug by geared pump; putting the mother liquid into finished product jug by gerared pump, mixing with dry compressed air for 0.5 hour; the rate of paraffinic base and 2,6-ditrertiarybutyl p-methylphenyl is 997-999:1-3.

Description

A kind of preparation method of paraffinic base softening oil

(1) technical field

The present invention relates to a kind of preparation method of paraffinic base softening oil.

(2) background technology

Usually select common lubricating oil when making butyl rubber inner tube and vulcanizer moulding for use, this oil ingredient complexity, cut is wide, it is more to contain unsaturated hydrocarbons, resistance of oxidation is poor, and volatility is big, but because the butyl rubber inner tube Working environment is more abominable, usually work under hot conditions, poor, the volatility Da Yi of lubricating oil resistance of oxidation causes tube aging like this.

(3) summary of the invention

At the problems referred to above, the invention provides a kind of preparation method of paraffinic base softening oil, it has good oxidization resistance and low volatility, and the process oil when can be used as the vulcanizer moulding, the butyl rubber inner tube of manufacturing have stronger antioxidant property, and work-ing life is longer.

Its technical scheme is such: it is characterized in that it may further comprise the steps,

A, modulation mother liquor:

A, a spot of paraffin base oil is sent in the blending kettle, and heat temperature raising to 65 ± 5 ℃, circulation while stirring if paraffin base oil is moisture, then allows to be heated to 100 ℃ and dewaters;

B, with in the 2.6-ditertbutylparacresol impouring blending kettle, stir with stirrer and toothed gear pump;

The modulation of B, processed oil:

A, the modulation mother liquor in, paraffin base oil is pumped into the finished product jar with toothed gear pump;

B, synthetic mother liquor is pumped into the finished product jar, simultaneously with exsiccant pressurized air mixing oil product with toothed gear pump; Mixed at least 0.5 hour, qualified back is to be packaged;

The ratio of total amount that paraffin base oil uses in above-mentioned A step, B step and 2.6-ditertbutylparacresol (T501) total amount is 997 to 999 to 1 to 3.

Among the present invention, because the paraffin base oil cut of selecting for use narrow (lighting end content is low), saturated hydrocarbon content height (unsaturated hydrocarbons content is low), add oxidation inhibitor 2.6-ditertbutylparacresol again, so its good in oxidation resistance, volatility are low, the softening oil that processes has good oxidization resistance and low volatility, process oil when can be used as the vulcanizer moulding, the butyl rubber inner tube of manufacturing has stronger antioxidant property, and work-ing life is longer.

(4) description of drawings

Fig. 1 is a process flow sheet of the present invention.

(5) embodiment

Below in conjunction with Fig. 1 technological process of the present invention is described:

The modulation mother liquor is sent into a spot of paraffin base oil in the blending kettle, and heat temperature raising to 65 ± 5 ℃, and circulation while stirring if paraffin base oil is moisture, then allows to be heated to 100 ℃ and dewaters; Additive 2.6-ditertbutylparacresol (T501) in the whole impouring blending kettle in blending kettle top, after adding, is stirred with stirrer and toothed gear pump, and the mother liquor modulation finishes like this; Paraffin base oil is pumped into the finished product jar with toothed gear pump, and the mother liquor with the blending kettle internal modulation pumps into the finished product jar again, with exsiccant pressurized air mixing oil product, mixes at least 0.5 hour simultaneously, and qualified back is to be packaged; The mother liquor that stirring in blending kettle when the softening oil mass of making is less finishes forms detects and conforms with also can packing that softening oil requires.The process of above-mentioned making softening oil, no matter the few softening oil amount of still being that is processed in blending kettle of the amount of being pumps into mother liquor finished product jar post-treatment greatly again and becomes softening oil (paraffinic base) after blending kettle modulates mother liquor, the total amount that paraffin base oil uses and the ratio of 2.6-ditertbutylparacresol (T501) total amount are 997 to 999 to 1 to 3, and optimum proportion is 998 to 2; The paraffin base oil that uses among the present invention belongs to the market existing procucts, but its quality index need meet following condition, specifically sees Table 1,

Sequence number	Project	Quality index	Test method
				1	Kinematic viscosity (50 ℃) mm 2/s	24～32	GB/T265
2	Flash-point (opening) ℃ is not less than	200	GB/T267
				3	Water soluble acid or alkali	Do not have	GB/T259
4	Moisture, %	Do not have	GB/T260
				5	(170 ℃, 90min) % is not more than fugitive constituent	1.7	Appendix A
6	Hydrocarbon composition, % C ABe not more than C PBe not less than	10 60	Appendix B
				7	Pour point ℃ is not higher than	0	GB/T3535
8	Aniline point ℃ is not less than	98	GB/T262

Annotate: appendix A and appendix B ask for an interview the back appendix.

Appendix A

(standardization appendix)

The mensuration of fugitive constituent

A1 instrument and material

A. furnace pot: Φ 80,75ml

B. moisture eliminator

C. enamel sample disc with cover

D. thermostat container: sensitivity ± 1 ℃, interior chamber vol 〉=300 * 300 * 300mm

E. crucible tongs

A2 preparation work

The sample (being no more than volumetrical 3/4) that a. will be contained in the container shakes 5min, mixes.

B. furnace pot is put into the beaker that dilute hydrochloric acid (1: 4) is housed, heated and boiled 5min takes out.Wash, move into dry (the not air blast) in 1 hour that (be placed on the baking oven upper strata) in 170 ± 1 ℃ the thermostat container, be placed on then and cool off 30min in the moisture eliminator, carry out weighing (claiming accurate) to 0.0002g by the thermometer place.The difference that drying and weighing operation repeat between double weighing is no more than 0.0004g.

The A3 testing sequence

A. taking by weighing 5～6g sample from the sample that mixes claims accurate to 0.0002g in the furnace pot of constant weight.

The furnace pot that b. will fill sample is positioned in the sample disc (does not add a cover), moves into (170 ± 1 ℃) in the adjusted good thermostat container, and constant temperature 90min moves into furnace pot in the moisture eliminator then, and cooling 30min carries out weighing, claims accurate to 0.0002g.

A4 calculates

The fugitive constituent X% of sample presses column count:

$X=\frac{G_1-G_2}{G}\×100\%$

In the formula: G ₁---the weight of sample and furnace pot before the volatilization test, g;

G ₂---the weight of test back sample and furnace pot, g;

G---example weight, g.

A5 precision

Difference between two results of average measurement should not surpass 0.1%.

The A6 report

The arithmetical av that is averaged two results of mensuration is as test-results.

Appendix B

(standardization appendix)

The mensuration of hydrocarbon composition

Test method with carbon distribution and building stone analysis in the n-d-M method mensuration petroleum oil.

The B1 scope

B1.1 present method relates to the non-olefinic oil, calculates carbon distribution and ring content by measuring refractive index, density and molecular weight (n-d-M).(annotating 1)

Annotate 1: the composition of petroleum mixture often is expressed as umber, distribution aromatic ring part (R _A) alicyclic moiety (R _N) and paraffin chain portion (R _P) they are all by imagination, or include the molecule of a desirable meaning, in addition, composition can also represent that promptly the percentage ratio of total carbon atom is divided into aromatic ring structure (%C by carbon distribution _A), alicyclic structure (%C _N), paraffin bond structure (%C _P).

B2 method summary

The refractive index of oil and the mensuration of density are all at 20 ℃, and the mensuration of molecular weight can be used empirical method, also can measure the viscosity of 100 and 250 (38.7 ℃ and 100 ℃) and calculate these data, then, are used as and calculate carbon distribution (%C _A, %C _N, %C _P).

B3 purposes and utilization

Carbon distribution and ring content can be used for representing the importance score of the rough composition of oil, these data are when making the base oil of lubricating oil, can be as the auxiliary monitoring of overall performance, these manufacturing processedes can be the refining or hydrogenation of solvent distillation, the base oil that maybe will come from different crude oils mixes, even these data also the method research through being commonly used for curve and the relation between product importance.

The measurement of B4 physicals

Refractive index (the n of B4.1 oil _D) when 68 °F (20 ℃), measure by Abbe refractometer.

Density (the d of B4.2 oil ₄) when 68 °F (20 ℃), press GB1884 oil and liquid petroleum product densitometry.

The sulphur content of B4.3 oil is pressed GB387-64 (82) and is measured.

The calculating of B5 carbon distribution and ring content

B5.1 calculated factor X and Y are by the density (d that measures ₄) and observe refractive index (n _D) calculate with following formula:

X＝2.51(n _D-1.4750)-(d ₄-0.8510)

Y＝(d ₄-0.8510)-111(n _D-1.4750)

B5.2 molecular weight M records kinematic viscosity V by 37.8 ℃ and 98.9 ℃ _37.8And V _98.9Calculate.

(1)H _37.8＝870loglog(V _37.8+0.6)+154

(2)H _98.9＝870loglog(V _98.9+0.6)+154

(3)W＝4.146-1.733log(H _37.8-H _98.9-145)

(4)M＝W(H _37.8+0.6)+180

Annotate: W is a calculated factor herein.

B5.3 calculates aromatic ring carbon percentage composition from X and molecular weight (M) with following formula:

As X is positive %C _A=430X+3660/M

X is negative %C _A=670X+3660/M

B5.4 calculates the percentage amounts (%C of total ring (aromatic ring and alicyclic ring) structure with following formula with Y and molecular weight _R).

As Y is positive %C _R=820Y-3S+1000/M

If Y is negative %C _R=1440Y-3S+10600/M

Annotate: S is the weight percentage of sulphur herein.

B5.5 paraffin carbon percentage amounts is calculated with following formula:

％C _P＝100-％C _R

The B6 accuracy

The tolerance range that B6.1 present method is obtained is added up in the laboratory, and its result is as follows:

The a circulation ratio is by same operator, and same instrument carries out repeatedly successful test in identical operations condition and same test materials, and the difference that may cause, in the value that in 20 times, exceeds following table under these standards and the correct operation below once:

The scope repetition rate

%C _A2.7 to 34.6 0.6

%C _N23.7 to 47.7 1.2

%C _P32.3 to 68.6 1.0

R _A0.12 to 1.69 0.04

R _N1.61 to 2.90 0.08

R _T1.13 to 3.77 0.08

Difference between the single separate result of one or two of b reproducibility by the same appointment test materials in different laboratories, is carried out repeatedly test by standard and correct test method, and scope exceeds the value of following table below once in 20 times:

The scope repetition rate

%C _A2.7 to 34.6 1.7

%C _N23.7 to 47.6 3.6

%C _P32.3 to 68.6 3.4

R _A0.12 to 1.69 0.09

R _N1.61 to 2.90 0.23

R _T1.73 to 3.77 0.23

Claims (1)

1, a kind of preparation method of paraffinic base softening oil, it is characterized in that: it may further comprise the steps,

A, modulation mother liquor:

A, a spot of paraffin base oil is sent in the blending kettle, and heat temperature raising to 65 ± 5 ℃, circulation while stirring if paraffin base oil is moisture, can be heated to 100 ℃ and dewaters;

B, with the 2.6-ditertbutylparacresol in the whole impouring blending kettle in blending kettle top, stir with stirrer and toothed gear pump;

The modulation of B, processed oil:

A, the modulation mother liquor in, paraffin base oil is pumped into the finished product jar with toothed gear pump;

B, synthetic mother liquor is pumped into the finished product jar, simultaneously with exsiccant pressurized air mixing oil product with toothed gear pump; Mixed at least 0.5 hour, qualified back is to be packaged;

The total amount that paraffin base oil uses in above-mentioned A step, B step is 997 to 999 to 1 to 3 with the ratio of 2.6-ditertbutylparacresol total amount.