CA1138801A - Treatment of coal tar with ethoxylated sulfated surface-active compositions - Google Patents

Treatment of coal tar with ethoxylated sulfated surface-active compositions

Info

Publication number
CA1138801A
CA1138801A CA000363232A CA363232A CA1138801A CA 1138801 A CA1138801 A CA 1138801A CA 000363232 A CA000363232 A CA 000363232A CA 363232 A CA363232 A CA 363232A CA 1138801 A CA1138801 A CA 1138801A
Authority
CA
Canada
Prior art keywords
tar
water
mixture
treatment
coal tar
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
Application number
CA000363232A
Other languages
French (fr)
Inventor
Samuel Cukier
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Domtar Inc
Original Assignee
Domtar Inc
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Domtar Inc filed Critical Domtar Inc
Priority to CA000363232A priority Critical patent/CA1138801A/en
Priority to ZA817226A priority patent/ZA817226B/en
Priority to AU76661/81A priority patent/AU546514B2/en
Priority to JP56169389A priority patent/JPS57177088A/en
Priority to EP81850196A priority patent/EP0051056B1/en
Priority to DE8181850196T priority patent/DE3169195D1/en
Priority to ES506517A priority patent/ES8205849A1/en
Application granted granted Critical
Publication of CA1138801A publication Critical patent/CA1138801A/en
Expired legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10CWORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
    • C10C1/00Working-up tar
    • C10C1/02Removal of water

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Working-Up Tar And Pitch (AREA)
  • Solid Fuels And Fuel-Associated Substances (AREA)
  • Coke Industry (AREA)

Abstract

TREATMENT OF COAL TAR
WITH ETHOXYLATED SULFATED SURFACE-ACTIVE COMPOSITIONS
ABSTRACT
The present invention relates to a process for the treatment of coal tar comprising thoroughly mixing the coal tar with a surface-active composition, followed by a separation of water and quinoline insoluble components from the mixture.

Description

11388~S~

Field of the Invention The present invention relates to bituminous mate-rial. More particularly, it relates to a method for modify-ing coal tar material.
Background of the Invention / Pri r Art The water content of coal tars is one of its more variable and troublesome characteristics. Associated with this water content are ammonium compounds, in particular ammonium chloride, to which much of the equipment corrosion during tar distillation can be attributed. While the addi-tion o alkali to the tar will reduce the corrosion, the usually non-volatile alkali compound remains in the pitch residue following distillation, often affecting its proper-ties adversely.
Attempts have been made, with varying degrees of success to eliminate or diminish the water content of the tar. The less successful ones have included addition of electrolyte, modification of the tar pH, freezing of the tar, and subjecting the tar to high frequency mechanical agitation. Among the more successful processes has been boiling the tar. Nonetheless such a procedure is rather energy intensive and generally fails to achieve an adequate reduction in the water content of the tar.
Another problem that has plagued the users of tar is the often high (and also variable) content of quinoline insolubles (Q.I.) therein. The problem is particularly noticeable when these insolubles are concentrated in the pitch residue following the distillation of the tar. The particulate nature of Q.I. renders difficult virtually any process which re~uires the passage of the pitch through small orifices, eg. in the impregnation of porous, baked carbon bodies. Additionally, should the Q.I. have a high inorganic portion, the combustion rate of the carbon body ~138~

produced by coking (or otherwise carbonizing) the pitch will be si~nificantl~ increased.
~ ccordingly, it is an object of this invention to provide an improved process for the dewatering of tars.
It is also another object of this invention to de-crease the quinoline insoluble content in the tar.
Brief Description of the Invention The process for treating coal tar material con-taininq water and quinoline insolubles, comprising: mixing a surface active composition with said material so as to facilitate the segregation of at least a portion of at least one of said water and said quinolir.e insolubles from said tar where said surface active composition contains as the active ingredient, a member chosen from the group comprising the class of compounds having the general Eormula CH3(CH2)XCH2(OCH2CH2)yOSO3~M+, where the average value of x lies in the range 6.5 to 13, y is at least 1.5, and M+ re-presents one of sodium and ammonium ions~
; Detailed Description of the Invention Accordingly, the present invention relates to a process whereby a bituminous material, in particular coal tar, can be treated in order to decrease the amount of water and quinoline insolubles contained therein. Broadly stated, this process will comprise the steps of thoroughly mixing the tar with a surface-active composition defined below, so as to facilitate the segregation of at least one of the water and the quinoline insGlubles from the mixture, which can be subsequently separated from the muxtures. The surface-active composition used herein will comprise a member chosen from the class of compounds having the general formula CH3(cH2)xcH2(ocH2cx2)yoso3-Ml; where the average value of x lies in the range 6.5 to 13, y is at least 1.5 and M~ represents one of sodium and ammonium ions. For ~1388~
example, a particularly efficacious composition for use herein is the ethoxylated sulfate prepared from the C13 al-cohol, ie. x = 11 in the above terminology. Clearly indi~
vidual values of x can lie within or outside these bounds.
The ethylene oxide portion will usually constitute about 40%
of the molecular weight, which will correspond to y taking on values in the range 1.5 to 6. The amount of surface-active composition which will be employed will usually range from about 0.001 to 1% of the coal tar material, although quantities which fall outside these limits may also be used, depending on the material being treated and the end-result sought.
Procedurally, the present invention will comprise mixing the surface-active composition with the tar at a tem-perature where the tar is in a relatively fluid state, in any event stirrable or pumpable (typically about 70-90C).
For example, the surface-active composition may be bled in while the tar is being pumped into a storage tank, thus uniformly distributing the additive throughout the tar while obviating the need for any special mixing equipment.
The mixture is maintained at the stirrable tem-perature while the ensuing separation is carried out. It should be noted, however, that an increase in temperature can improve the separation, but may lead to some modifica-tion of the constituents of the tar. The separation may be carried out, for example, merely by leaving the mixture in a quiescent state while permitting the water and solids to separate as the top and bottom strata of the mixture, which may be subsequently separated from the tar by means of decantation or the like. Alternatively, an improved separa-tion can be obtained if techniques such as centrifugation of the mixture are employed. The separation technique employed will, in part, determine the degree to which water and ~1388~

quinoline insolubles will be separated from the tar.
While it is not entirely clear how the addition of the surface-active compo~ition can cause a separation of both the quinoline insoluble and the water from the tar; it is believed that the water and the quinoline insoluble content of the untreated material are somehow associated with each other so as to form a disperse phase having an ap-parent density which is substantially the same as that of the tar. The addition of the surface-active agent causes these components of the disperse phase to dissociate and rise or sink in the body of tar according to their respec-tive specific gravities relative to tar. A desirable at-tribute of the present process is the substantial absence of residual surface-active agent in the tar following the sepa-` ration of the tar from the water, since the surface-active agent will be associated with and removed with the water.
In addition to the removal of the water and Q.I. from the tar, the present invention generally removes salts, electro-lytic material and other inorganics associated with the Q.I. and the water which might result in an increased corro-sion during processing and an increased oxidation rate of the coke formed therefrom. However the actual mechanism whe~eby the addition of the surface-active agent affects the quinoline insolubles, water and/or the tar itself may be quite different from the hypothetical one outlined above and accordingly we would not wish to be restricted thereto.
- The following examples will serve to illustrate some embodiments of the present invention.
Example 1 The heavy tar which was to be subjected-to the process of the present invention was first mixed with an ethoxylated sulfated ester salt of fatty alcohols having an average chain length of 13 carbon atoms (in the above ~13880~

terminolog~ where x = 11), and an average value ~f y = 2.2, approximately. The mixing of tar with the surface active agent was carried out at about 8~-90C following which 2 samples of the tar mixture containing 0.1% by weight of this surace active agent were allowed to stand in ovens at tem-peratures of about 75 and 90C, respectively for about 24 hours, thus simulating the conditions of relative quiescence and temperature prevailing in a tar storage tank. The water - which separated at the surface was decanted off and measured while the residual water content of the tar was also mea-sured. The results, which indicate the proportions of the water separated by decantation and the water residual in the ; tar are indicated in Table I below. The small discrepancies i, in the total water contents before and after treatment are insignificant.
A water reducing agent for tars, commonly used in the industry, and which comprises a polypropylene oxide-type surfactant sold under the trademark ~Tretolite" was added to the tar in proportions which constituted 0.2% by weight of the resultant mixture. This mixture was divided into 2 por-tions and subjected to the same treatment as described above. The residual water content of the tar were ~easured and was found substantially unchanged. These results which are summarized in Table I below, indicate that recourse to the present invention results in a better separation of the water from tar.
In a similar experiment, tar having an augmented water content (about 18.4% by weight of the tar-water mixtu-re) was prepared and two samples from this mixture were treated with about 0.1% by weight of the present invention surface-actiYe agent, and 0.2% by weight Tretolite (TM).

The samples were placed in an oven set at 90C. Following 24 hours of this treatment r the separated and residual water 113~
contents of the tar were determined for each of the samples, and are summarized in table I below. As before, notwith-standing the smaller amounts of surface active agent employ-ed, the present invention results in better water removal from the tar.
TABLE I

Present Inven- ~
' ' tion Surface- ' 0.2% Tretolite ' ' Active Agent , (TM) _ _ _ ' Water ' Water ' Tar as Water Remain-'Water Remain-. Received.Decanted ing .Decanted ing 'after 24 after 'after 24 after 'hr. 24 hr. 'hr. 24 hr.
(%) I (%) (%) (%) (%) Water .. _ ~_ ._._ Tar Sample ¦ 9.0 ¦ j 24 hrs. at 75C ' ' 2.2 6.4 ' Nil 8.5 24 hrs. at 90C ' 5.0 3.5 ' Nil 8.0 Tar Sample + 10%i Water mixed in ' 18.4 30 After 24 hrs.
at 90C ' ' 13.5 4.0 . 5.0 12.5 Example 2 While the present invention can be successfully employed with tars having a high Q.I. content, it can also be applied to tars having a relatively low Q.I., as this example demonstrates.
Accordingly, tar samples having a Q.I. content of 7.3% and containing 0.1% by weight of the same surface-active agent employed in the preceding example were pre-pared. Equal proportions of untreated and treated tar were spun at a high speed tabout 1000 r.p.m.) on a clinical cen-trifuge for 5 minutes at 70, 80 and 90C. The Q.I. of the overflow fraction of the centrifuged material was measured, and is summarized in Table II below. It will be evident upon an examination of the table that the decrease in the ~388~

Q.I. ranges from between about 20 - 25%, and the overflow fraction from the higher temperature centrifugation could be used in the preparation of an impregnating pitch.

TABLE I I
Centrifugation Temperature ' ' 90C ~ 80C 5 70C
. , % Q.I. in the overflow fraction Untreated ' I ~ i Tar , 4.1 ' 4.3 ' 4.6 'Treated iTar i 3-1 5 3.3 j 3.6 The overflow (of about 85%) from the two samples of tar (i.e. untreated and treated) which had been centri-fuged at 90C, were subjected to filtra~ion carried out at 90C and under a nitrogen pressure of 75 p.s.i.g. The pro-portion of the tar sample that passed through the filter in the first minute was about 54~ in the case of the untreated tar and 62~ in the case of the treated tar. The reason for the easier filtration of the treated tar include the pres-ence of a smaller amount of solids, and a lower tar viscosi-ty due to the treatment.
Example 3 This example illustrates how the additior. of the surface-active agent of the present invention to the tar and allowing the tar to stand as described in the present inven-tion can result in a marked stratification of some of the components therein, eg. the Q.I., free carbon and water and comparing their concentrations in the untreated tar which is homogeneous due to the stability OL the water-Q.I. emul-sions.
0.1% of surface-active agent was mixed with the tar at 85C, samples taken from the middle and bottom strata and tested for their Q.I., free carbon and water contents, 1138~

after the tar had been allowed to stand for about 4.5 hours. This procedure was repeated after a standing time of 28 hours. The results Gf these tests as well as values of Q.I., free carbon and the water content in the untreated tar are summarized in Table III below.
The entries in the table below demonstrate how the treatment serves to increase the free carbon and the Q.I.
content of the bottom layers while reducing the water content therein from 17.3 to 2%. Obviously, the decrease in the water content of the lower strata will be balanced by an equivalent increase in the upper strata from which it can easily be removed.
TABLE III

. . Untreated ' Middle ' Bottom Tar , Stratum , Stratum (%) i (%) ' (%) . . .
' Quinoline 5 , Insoluble , 0 hrs . 14.3 ' 14.3 ' 14.3 4.5 " , 14.8 , 15.9 2B " ' '16.0 ' 16.1 i Free Carbon, 0 hrs ' 20.8 ' 20.8 ' 20.8 ' ' 4.5" ' ,23.1 '24.6 j j 28" j '22.7 '24.8 Water ' 0hrs ' 17.3 '17.3 ,17.3 ' ' 4.5" . .3.0 .3.0 j 1 28~ j j2.0 j2.0 . ~
The description and examples provided above are for the purpose of providing a complete disclosure of the invention, and alterations and modifications within the scope of the amended claims, may occur to those skilled in the art.

Claims (7)

CLAIM
1. A process for treating stable emulsions of coal tar material containing water and quinoline insolubles, comprising mixing a surface active composition with said material in an amount effective to facilitate the segregation of at least a portion of at least one of said water and said quinoline insolubles from said mixture, where said surface active composition is chosen from the class of compounds having the general formula CH3(CH2)xCH2 (OCH2CH2)yOSO3-M+ where the average value of x is in the range 6.5 to 13, y is at least 1.5, and M+ represents one of sodium and ammonium ions.
2. A process as defined in Claim 1, wherein said segregated portion of at least one of said water and said quinoline insolubles is separated from said mixture.
3. A process as defined in Claim 1, wherein y is at most 6.
4. A process as defined in Claim 2 wherein said separation is carried out by decantation of said mixture.
5. A process as defined in Claim 2 wherein said separation is carried out by centrifugation of said mixture.
6. A process as defined in Claims 2, 3 or 4 wherein said separation is carried out at a temperature greater than 70°C.
7. A process as defined in Claims 2, 3 or 4 wherein said surface-active composition is added to said coal-tar material in an amount which constitutes between 0.001 and 1% of said coal-tar material.
CA000363232A 1980-10-24 1980-10-24 Treatment of coal tar with ethoxylated sulfated surface-active compositions Expired CA1138801A (en)

Priority Applications (7)

Application Number Priority Date Filing Date Title
CA000363232A CA1138801A (en) 1980-10-24 1980-10-24 Treatment of coal tar with ethoxylated sulfated surface-active compositions
ZA817226A ZA817226B (en) 1980-10-24 1981-10-19 Treatment of coal tar
AU76661/81A AU546514B2 (en) 1980-10-24 1981-10-20 Separation of water and/or quinoline insolubles from coal tar
JP56169389A JPS57177088A (en) 1980-10-24 1981-10-22 Coal tar treatment
EP81850196A EP0051056B1 (en) 1980-10-24 1981-10-23 Treatment of coal tar
DE8181850196T DE3169195D1 (en) 1980-10-24 1981-10-23 Treatment of coal tar
ES506517A ES8205849A1 (en) 1980-10-24 1981-10-23 Treatment of coal tar.

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CA000363232A CA1138801A (en) 1980-10-24 1980-10-24 Treatment of coal tar with ethoxylated sulfated surface-active compositions

Publications (1)

Publication Number Publication Date
CA1138801A true CA1138801A (en) 1983-01-04

Family

ID=4118257

Family Applications (1)

Application Number Title Priority Date Filing Date
CA000363232A Expired CA1138801A (en) 1980-10-24 1980-10-24 Treatment of coal tar with ethoxylated sulfated surface-active compositions

Country Status (7)

Country Link
EP (1) EP0051056B1 (en)
JP (1) JPS57177088A (en)
AU (1) AU546514B2 (en)
CA (1) CA1138801A (en)
DE (1) DE3169195D1 (en)
ES (1) ES8205849A1 (en)
ZA (1) ZA817226B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4744882A (en) * 1987-01-02 1988-05-17 Domtar Inc Polycondensates of sulfonated coal tar fractions

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5812160B1 (en) * 2014-06-09 2015-11-11 栗田工業株式会社 Coal tar oil / water separator and coal tar oil / water separator
JP6350025B2 (en) * 2014-06-26 2018-07-04 栗田工業株式会社 Oil-water separation method and oil-water separation agent for oil-containing scum or oil-containing wastewater
JP5962784B2 (en) * 2015-01-13 2016-08-03 栗田工業株式会社 Oil-water separation method and oil-water separation agent for hydrous coal tar

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1010972B (en) * 1955-01-12 1957-06-27 Henkel & Cie Gmbh Process for the separation of mixtures of solid crystallizable and liquid substances found in tars
AU492350B2 (en) * 1974-07-29 1976-01-29 Texaco Development Corporation Demulsification compositions
US4139451A (en) * 1977-12-12 1979-02-13 Nalco Chemical Company Method for dewatering coke tar-water mixtures
US4277352A (en) * 1979-03-26 1981-07-07 Texaco Inc. Demulsification of emulsions produced from surfactant recovery operations and recovery of surfactants therefrom

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4744882A (en) * 1987-01-02 1988-05-17 Domtar Inc Polycondensates of sulfonated coal tar fractions

Also Published As

Publication number Publication date
AU7666181A (en) 1982-04-29
ES506517A0 (en) 1982-08-16
EP0051056B1 (en) 1985-03-06
DE3169195D1 (en) 1985-04-11
ES8205849A1 (en) 1982-08-16
AU546514B2 (en) 1985-09-05
JPS57177088A (en) 1982-10-30
EP0051056A1 (en) 1982-05-05
JPH0119439B2 (en) 1989-04-11
ZA817226B (en) 1982-09-29

Similar Documents

Publication Publication Date Title
DE69016623T2 (en) Silicone antifoam.
DE2724187A1 (en) PROCESS FOR FOAM CONTROL IN NON-Aqueous SYSTEMS
CA1138801A (en) Treatment of coal tar with ethoxylated sulfated surface-active compositions
US5215669A (en) Use of mixed hydroxyethers as auxiliaries for the dehydration of solids
US4395326A (en) Treatment of coal tar emulsions
US1375811A (en) Fuel and method of producing same
DE2451969C2 (en) PROCESS FOR GLAZING WORKPIECES MADE OF CERAMIC, CHARCOAL OR CARBON
DE1082453B (en) Fuel for jet engines
EP0283584B1 (en) Process for reducing the water and ash content in crude tar
US1819070A (en) Process for chemically impregnating jute sacks, tent cloth, and the like
SU1083914A3 (en) Method for treating stable emulsions of coal tar
EP0117383B1 (en) Oxidation-resistant pitches
CA1142114A (en) Method of inhibiting precipitation of asphaltenes
US3135681A (en) Method of dewatering tar
US3151083A (en) Lubricating oils
RU2055945C1 (en) Anode mass production method
US2853430A (en) Process for stabilizing furnace oil
US2051255A (en) Manufacture of green bloom lubricating oils
DE686980C (en) Process for the production of low-ash or ash-free coal-oil dispersions
US1703239A (en) Arthur m
CN115725322A (en) Pretreatment method of coal tar
US2024117A (en) Method of treating and purifying motor fuels
US1878650A (en) Process for clarification of hydrocarbons containing suspended or colloidal complexes
SU1117307A1 (en) Method of cleaning coal tar
KR810001011B1 (en) Separation of solid from coal liquids using an additive

Legal Events

Date Code Title Description
MKEX Expiry