Process for purification of liquid sulphur from hydrogen sulphide and its polysulphides

专利摘要:
The invention relates to methods for the removal of hydrogen sulfide and its polysulfides from liquid sulfur and reduces the duration of the process. Sulfur is cleaned at 135-165 ° C with stirring while simultaneously blowing the free surface of sulfur with an inert gas. The process is carried out in the presence of a catalyst. The invention relates to methods for removing hydrogen sulfide contained in liquid sulfur in a dissolved or in a state linked to polysulfides. The aim of the invention is to reduce the duration of the process. The drawing is a diagram of the implementation of the method. It is a mixture of an alkaline agent with a surface-active substance (surfactant) or surfactant having basic properties. The alkaline agent is used in a mixture with a surfactant selected from the group consisting of ethoxylated alkyl phenols, oxyethylated alkyl mercaptans, oxyethylated fatty alcohols, oxyethylated fatty acids, fatty amides, oxyethylated fatty amides in which the fatty radical contains C 1O-Sc8. Fatty amines, alkylenediams, oxyethylated fatty amines, oxyethylated alkylenediamines, quaternary ammonium compounds with aliphatic chains, and benzalkonium salts are used as surfactants with basic properties. The catalyst is introduced in the amount of 0.5-1 May. hours at 1000 ma.ch. sulfur. The alkaline agent is introduced in an amount of 0.2-20% by weight of the catalyst. The process is carried out for 22-168 minutes. Residual content of pta. 3 hp f-ly, 1 ill., 1 tab. According to the proposed method, the purification of liquid sulfur from these compounds is carried out at 135-165 ° C with stirring while blowing the free surface of sulfur with an inert gas in the presence of a catalyst, which is a mixture of an alkaline agent or a surfactant substance with basic properties. iS (L oe N3 oo 00 01 GO cm
公开号:SU1628853A3
申请号:SU884355368
申请日:1988-03-09
公开日:1991-02-15
发明作者:Морис Жан；Фук Ромен；Ориоль Жан-Луи
申请人:Сосьете Насьональ Елф Акитэн /Продюксьон/ (Фирма)；
IPC主号:

专利说明:

The alkaline agents used are alkali or alkaline earth metal hydroxides, or such compounds, kakammiak, hydrazine, hydroxyl-amine, aliphatic or cyclic amines of primary, secondary or tertiary type, urea, thiourea and their derivatives, nitrogen-containing compounds, differing at operating temperatures with separation ammonia or amine.
The alkaline agent is used in a mixture with a surfactant selected from the group containing ethoxylated alkyl mercaptans, oxyethylated alkyl phenols, oxyethylated fatty alcohols, oxyethylated fatty acids, fatty amides, oxyethylated fatty amides, in which
The following compounds are used as surfactants with alkaline properties:
A) fatty propylenediamine formula
R-NH (CII2) 3-NHZ, where R is an aliphatic radical.
C2 °,,
B) N, N, H -Polyoxyethylene-K-fatty propylenediamine (PgPORAM S7) of formula
(fiu} MMSN2CH20) XH R K (CH2) 3 NN}
(CH2CH20) z-Ha
v
g
where R is the aliphatic radical C o and x + y + z 7;
B) polyoxyethylenated fatty amine (NORAMOX S7) of formula
R-KC
(СН2СНгО) х-Н
(Sn2sn2o) an
where R is the aliphatic radical and
D) polyoxyethylenated fatty amine (NORAMOX S5), similar to B, but with (x + y) 5;
L) N-bis-2-hydroxyethyl-cocoamine (NORAMOX C2) of the formula
R-M:
CH2CH2OH
CH2CH2OH
where R is the aliphatic radical C 0 -Cfg; E) di-costilamine NORAM M2C formula
R
: K-CH3
l
. where R is the aliphatic radical G) chloride di (hydrogenated fat) di-, methyl ammonium (.NORAMTIM M2SH) of formula
R / CH3
C1
where R is an alkyl radical with 3) dimethylbenzalkonium chloride of the formula -
in-SNS.
sg
0

five
0
five
0
five
The catalyst is introduced in the amount of 0.5-60.0 wt.h. per 1000% by weight. Sulfur sulfur at one time or in small portions.
In this case, the alkaline agent and the PVA are introduced in liquid sulfur together or separately.
The proposed method is carried out under conditions that ensure a homogeneous distribution of the catalyst and the removal of the precipitated. Such conditions are the mixing and stripping of HgS gas inert to this system: nitrogen, CO, air, water vapor, etc.
Example. The method is carried out in a closed heat-insulated chamber 1, divided into compartments 2 and 3 with a partition 4, open in the upper part, which allows liquid sulfur to be drunk from compartment 2 to compartment 3. The bottom 5 of compartment 2 is located above the bottom 6 of compartment 3. The chamber 1 is provided with a purge gas supply 7 entering the compartment 2 above the overflow level, and a purge gas outlet 8 located in the upper part of the compartment 3. In addition, the compartment 2 is on one side provided with a pipeline 9 for supplying liquid sulfur, and the pipeline 9 has a branch vie 10
516
for catalyst input. On the other hand, in the compartment 2, a mechanical mixing means 11 is installed.
The compartment 3 is provided with a means for spraying liquid sulfur 12, which includes a pump 13, the suction pipe 14 of which is immersed in liquid sulfur, and the discharge pipe 15 is connected to a nozzle 16 located in the compartment 3 above the free surface 17 of liquid sulfur in this compartment.
(The sulfur containing catalyst is agitated in compartment 2, which leads to a uniform distribution of the catalyst in liquid sulfur and initiation of the sulfate decomposition reaction. Then the liquid sulfur through partition 4 flows into compartment 3, where it is pulverized. is removed by circulating the purge gas, the mixture of which is directed to the combustion zone.
The method can be carried out continuously in a chamber divided into at least 3 consecutive separations.
The specific conditions of the embodiments of the method and their results are presented in the table.
As follows from the table, the use of the proposed catalysts allows reducing the duration of the processes from 300 min of the prototype to 22-170 min.

权利要求:
Claims (4)
[1]
1. A method for purifying liquid sulfur from hydrogen sulphide and its polysulfides, which includes heat treating it at 130-165 ° C in the presence of a catalyst, a grinding agent, with stirring and blowing off, the separated hydrogen sulphide from the sulfur surface with an inert gas, characterized in that A mixture of an alkaline agent with a surfactant selected from is used as a catalyst. groups containing ethoxylated alkyl mercaptans, ethoxylated alkylphenols with 12, ethoxylated fatty alcohols, ethoxylated fatty acids, fatty amides, ethoxylated fatty amides, in which the fatty radical contains
C1 (J-Cfg, or as a catalyst, a surfactant is used which has alkaline properties and is selected from the group containing fatty amines of the general formula
K2
or their salts, alkylenediamines of the general formula
R-NH- (CmH2n,) - NH,
in the form of their salts, ethoxylated fatty amines of the general formula
15
R-N:
(CH2-CH2-0) X-H (CH2-Cig-0) y-H
20
hydroxyethylir and other general formulas
alkylenediamines
R-r (cmH2m} -N: Lc -5- "
(CH2-CHZ-Q) Z-H
(CH2-CH2-Q) y-H
25
quaternary ammonium compounds with aliphatic chains of the general formula
four
RxNx / 1X
benzalkoni salts of the formula
35
K7
0
five
0
where R is an alkyl or alkenyl radical with Cf0-C2 ();
R and E2 - radical R, hydrogen, methyl or ethyl radical;
Vrf
And Rg-R7 X
five
methyl or ethyl radical; and Y-anion chloride or acetate;
m 2,3,4; x, y, z - 1 ... 10.
[2]
2. A method according to claim t, characterized in that the alkaline agent is introduced in an amount of 0.2-20% by weight of the catalyst.
[3]
3. The method according to claim 1, characterized in that the alkaline agent
and the surfactant is introduced into the liquid sulfur in the mixture either separately.
716288538
[4]
4. The way popt. 1-3, otli-injected in an amount of 0.5-60.0 May, h.
due to the fact that the catalyst is at 1000 mas. sulfur.
Missing
140
NaOH in the form of a 3% solution in n-decanol
Oxyethylenated t-dodecyl mercaptan containing 7 units (OCH2CH2) 7 and 3% NaOH, 46 ppm NH5 (prototype)
Oxyethylenated nonylphenyl with 7 units (СН2СНгО) in which 0.6 wt.% NaOH, 30 ppm is dissolved. Catalyst 135 A
Catalyst
R
30 pounds 165
Catalyst
AT
 49 pounds
Catalyst L
ABOUT
30 60 90
20
ABOUT
thirty
60
90
20
ABOUT
thirty
70
95
20
145 133 120 113 103 136 128 118 108
96 473
67
31
18 8.5
ABOUT
60
20
40
00
ABOUT
15
thirty
40
45
465
284
132
18
9.5
150
74
25
9
five
ABOUT
6
18
20
ABOUT
four
12
thirty
five
8 o 4
12 20
About 5
452
33
four
-with.
504
274
173
122
78
2
477
83
eight
“And 508 103
and
1628353
I
T
2
moni, 45 h for 1000 h. of sulfur
Decanol 8150 (03) containing 4 wt.%
KOH, 25 parts per 1000 hours sulfur
Oleic acid - I40 lot 15 (03), containing 10% hexylamine,
30 hours for 1000 hours of sulfur
Stearic 150 acid 10 (OE), containing 6% octylamine,
15 hours for 1000 hours of sulfur
Laurilova acid - 150 lots 12 (03), containing
3 wt.% NaOH, 28 parts per 1000 hours of sulfur
v Dekanova Kis-140
Lot 8 (03) containing
4% by weight KOH, 20 h for 1000 h. Sulfur
Decanamide, 165 containing
3 wt.% NaOH, 35 h per 1000 hours of sulfur
Stearamide, 150 containing
5% by weight of urea, 38 hours, for 1000 hours of sulfur
Oleamide containing 150
10% NH4 carbonate, 40 parts per 1000 parts sulfur
Lauramide containing 140
3 wt.% NaOH, 30 parts per 1000 hours of sulfur
9 Stearamid 8 150 (03), containing 12 Continued Table
...
160
55 17 8.5
150
48
 sixteen
five



195
92
28
17
6
142
52
12
6
165 85 32
 ten
160
82
22
9
140
42
13
7
155
70
13 162885314
Table continuation
. -J
containing 4 wt.% 502t
KOH, 25 hours on 607 1000 hours sulfur
30 Decanamide 12 150 O150 (OE), containing 2036 th 3 but 3 percent by weight 3818 hydroxides of 475 tetrabutylammonium, 35 parts per 1000 parts of sulfur
31С10Н2 -МН- 1500430 (, tO40 40 hours for 2016 1000 hours of sulfur. 356
32С, бН37-Ш- 1400450 (СНг) г-Шг, 1630 30 h at 3017 1000 h. Sulfur 387
33C10HZ, -NH-1500420 (CHZ) -NH2 HC1.1535
35 hours to 3021
1000 hours of sulfur 428
34С, 1500445 (СН2) 31052 NH4CH3COOH, 2530 30 hours na429 1000 hours sulfur
35Cocodiethyl 1500490 amine .1062
(1 and 201
P-N 2 5287
To Ws
where R is the aliphatic radical with Cw — C 4g, 35 hours per 1000 hours of sulfur
36 Dodecylamine-1500455 hydrochloride, 1582 40 hours na 3021 1000 hours sulfur469
7 Dedilaminace- 1400440 tat, 20 hours to 1098 1000 h-, sulfur2545
8-.HCggSS
1072
30 hours to 2024
1000 hours of sulfur358
9 (enp) -n150 ° 45 °
Ttar sswцz
15
1628853
16 Continuation of the table

类似技术:

---

公开号 | 公开日 | 专利标题

---

SU1628853A3|1991-02-15|Process for purification of liquid sulphur from hydrogen sulphide and its polysulphides

---

RU2179949C2|2002-02-27|Sulfur degassing process and apparatus

---

PL184593B1|2002-11-29|Method of purifying gases

---

US4849204A|1989-07-18|Catalytic removal of hydrogen sulfides from liquid sulfur

---

US3953577A|1976-04-27|Process for purifying gases containing HCN

---

DE3269530D1|1986-04-03|A method for cleaning gas mixtures which might contain dust from a urea plant

---

US3975508A|1976-08-17|Method of prevention and removal of sulfur deposits from H2 S absorption equipment

---

GB1467083A|1977-03-16|Process and apparatus for the purification of coke oven gas

---

JPS58289A|1983-01-05|Removing method for hydrogen sulfide and hydrogen cyanide from gas liquor

---

JPS5594675A|1980-07-18|Method of processing drained water from coke production plant

---

JPS5721988A|1982-02-04|Removing method for cyanogen in gas liquor

---

DE407875C|1924-12-24|Production of sulfur, thiosulfates and sulfhydrates

---

GB2031864A|1980-04-30|Removing hydrogen sulphide from liquid sulphur

---

JPS59123599A|1984-07-17|Treatment of waste water containing nitrogenous sulfer compound and ammonia

---

US4209489A|1980-06-24|Apparatus for treating spent hydrochloric acid

---

SU1488249A1|1989-06-23|Method of producing elementary sulfur

---

DE964951C|1957-05-29|Process for the production of wetting agents, emulsifiers and detergents

---

SU190298A1|

---

PL152586B1|1991-01-31|The method of sodium and potassium thiocyanate decomposition

---

GB2054404A|1981-02-18|Improvements in or relating to foam filtering

---

RU92011369A|1995-10-10|METHOD FOR CLEANING GAS FROM HYDROGEN

---

RU95121236A|1997-11-27|METHOD FOR DEODORIZING CLEANING OF OIL AND GAS CONDENSATE FROM HYDROGEN SULPHIDE AND LIGHT MERCAPTANES

---

JPS58174293A|1983-10-13|Treatment of waste water

---

JPS5745395A|1982-03-15|Treatment of alkaline waste water containing sulfide by activated sludge

---

RU97106876A|1999-03-10|METHOD FOR CLEANING GAS CONDENSATE, OIL AND OIL PRODUCTS FROM HYDROGEN HYDROGEN

同族专利:

---

公开号 | 公开日

---

EP0252835B1|1990-11-07|

---

EP0252835A1|1988-01-13|

---

DK126488A|1988-03-09|

---

FI881114A|1988-03-09|

---

GR3001450T3|1992-09-25|

---

CA1300122C|1992-05-05|

---

FR2601351B1|1990-09-14|

---

ES2019649B3|1991-07-01|

---

FR2601351A1|1988-01-15|

---

DK168859B1|1994-06-27|

---

JP2511688B2|1996-07-03|

---

FI84337B|1991-08-15|

---

FI881114A0|1988-03-09|

---

NO173271B|1993-08-16|

---

JPH01500587A|1989-03-01|

---

NO173271C|1993-11-24|

---

NO881056L|1988-05-10|

---

WO1988000570A1|1988-01-28|

---

FI84337C|1991-11-25|

---

MX168373B|1993-05-19|

---

US4897251A|1990-01-30|

---

AT58110T|1990-11-15|

---

AU602712B2|1990-10-25|

---

US5004591A|1991-04-02|

---

DK126488D0|1988-03-09|

---

DE3766023D1|1990-12-13|

---

AU7701587A|1988-02-10|

---

NO881056D0|1988-03-09|

引用文献:

---

公开号 | 申请日 | 公开日 | 申请人 | 专利标题

---

---

US2838391A|1953-10-22|1958-06-10|Chemical Construction Corp|Method of treating sulfur bearing mineral values with molten sulfur to concentrate mineral sulfides|

---

US3447903A|1966-10-27|1969-06-03|Freeport Sulphur Co|Sulphur production|

---

US3664966A|1970-02-09|1972-05-23|Continental Oil Co|Dehydrohalogenation catalyst|

---

US3717600A|1971-01-13|1973-02-20|Merck & Co Inc|Magnesium oxide dispersions|

---

US4070383A|1975-02-18|1978-01-24|Ici Americas Inc.|Oxidative coupling of phenols and naphthols|

---

US4054605A|1975-04-17|1977-10-18|Texaco Development Corporation|Unsaturated amino alcohols|

---

DE2641108C2|1976-09-13|1978-05-18|Deutsche Gold- Und Silber-Scheideanstalt Vormals Roessler, 6000 Frankfurt|Accelerator combination for the crosslinking of powder coating binders|

---

US4393037A|1981-12-16|1983-07-12|Union Oil Company Of California|Method for reconditioning bacteria-contaminated hydrogen sulfide removing systems|

---

DE3417230A1|1984-05-10|1985-11-14|Metallgesellschaft Ag, 6000 Frankfurt|METHOD AND DEVICE FOR DE-GASIFYING LIQUID SULFUR WITH HYDROGEN|

---

DE3515709C1|1985-05-02|1986-12-18|Union Rheinische Braunkohlen Kraftstoff AG, 5000 Köln|Process for cleaning liquid sulfur|

---

FR2601351B1|1986-07-10|1990-09-14|Elf Aquitaine|PROCESS FOR THE RAPID REMOVAL OF HYDROGEN SULFIDE CONTAINED IN LIQUID SULFUR AND CATALYTIC SYSTEM FOR USE IN ITS IMPLEMENTATION.|

---

JPH081710A|1994-06-27|1996-01-09|Sankyo Kasei Co Ltd|Resin molding method|FR2601351B1|1986-07-10|1990-09-14|Elf Aquitaine|PROCESS FOR THE RAPID REMOVAL OF HYDROGEN SULFIDE CONTAINED IN LIQUID SULFUR AND CATALYTIC SYSTEM FOR USE IN ITS IMPLEMENTATION.|

---

CA2160412A1|1994-10-13|1996-04-14|Adolf Frederik Scheybeler|Method and apparatus for degassing sulphur|

---

US5807476A|1995-10-10|1998-09-15|United Laboratories, Inc.|Method of removing sulfur compounds from sour crude oil and sour natural gas|

---

AT405721B|1997-11-07|1999-11-25|Oemv Ag|DEVICE FOR SEPARATING GAS FROM LIQUIDS AND USE OF THE DEVICE FOR SEPARATING SULFUR HYDROGEN FROM LIQUID SULFUR|

---

US6656445B2|2000-10-13|2003-12-02|Baker Hughes Incorporated|Hydrogen sulfide abatement in molten sulfur|

---

US6583103B1|2002-08-09|2003-06-24|S.C. Johnson & Son, Inc.|Two part cleaning formula resulting in an effervescent liquid|

---

US7081233B2|2004-05-18|2006-07-25|Dynamax Engineering Ltd.|Method and apparatus for degassing liquid sulfur|

---

US7927577B2|2009-01-12|2011-04-19|Worleyparsons Group, Inc.|Sulfur collection systems and processes with integrated degassing|

---

FR2944456B1|2009-04-16|2011-05-06|Inst Francais Du Petrole|METHOD FOR DESULFURIZING A GASEOUS EFFLUENT HAVING AN ONLINE ANALYSIS AND CONTROL DEVICE|

---

US9346677B2|2012-08-29|2016-05-24|Sandvik Process Systems Llc|Sulfur degasser apparatus and method|

---

US9192887B2|2013-06-21|2015-11-24|Phillips 66 Company|Process for in-situ production of low dissolved hydrogen sulfide, degassed, sulfur from claus sulfur recovery|

---

WO2014204965A1|2013-06-21|2014-12-24|Phillips 66 Company|Process for degassing condensed sulfur from a claus sulfur recovery system|

---

US9573081B2|2013-06-21|2017-02-21|Phillips 66 Company|Process for degassing condensed sulfur from a claus sulfur recovery system|

---

US9758376B2|2013-06-21|2017-09-12|Phillips 66 Company|Process for degassing condensed sulfur from a Claus sulfur recovery system|

---

US9617154B1|2015-09-30|2017-04-11|Mahin Rameshni|Superdegas—a process of integrating sulfur collection and degassing for zero emission|

法律状态:

优先权:

---

申请号 | 申请日 | 专利标题

---

FR8610063A|FR2601351B1|1986-07-10|1986-07-10|PROCESS FOR THE RAPID REMOVAL OF HYDROGEN SULFIDE CONTAINED IN LIQUID SULFUR AND CATALYTIC SYSTEM FOR USE IN ITS IMPLEMENTATION.|

---