CN106185833B - The method that sulphur is detached from high sulfur Gas Fields gathering system solid deposits - Google Patents
The method that sulphur is detached from high sulfur Gas Fields gathering system solid deposits Download PDFInfo
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- CN106185833B CN106185833B CN201610775168.9A CN201610775168A CN106185833B CN 106185833 B CN106185833 B CN 106185833B CN 201610775168 A CN201610775168 A CN 201610775168A CN 106185833 B CN106185833 B CN 106185833B
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- sulphur
- solid deposits
- high sulfur
- gathering system
- gas fields
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/02—Preparation of sulfur; Purification
- C01B17/027—Recovery of sulfur from material containing elemental sulfur, e.g. luxmasses or sulfur containing ores; Purification of the recovered sulfur
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
Abstract
The present invention relates to gas gathering and transportation fields,More particularly to a kind of method detaching sulphur from high sulfur Gas Fields gathering system solid deposits,This method is after solid deposits are removed moisture removal and organic impurities using dryer,Solid deposits after drying are ground to the powder that average grain diameter is less than 200 microns,The solder(ing)acid that configuration quality percentage is 75%~85% at 60 DEG C,Solid deposits powder is placed in aforementioned solder(ing)acid,The smaller sulphur of density in deposit,Diatomite will float up to solution upper layer,Take upper layer suspended matter,It is placed in the liquor zinci chloridi that mass percent is 55%~65%,Diatomite will float on above aqueous solution,Sulphur will be deposited below aqueous solution,Pass through the second-order separation technique,Efficiently separating for sulphur in high sulfur Gas Fields gathering system solid deposits may be implemented.
Description
Technical field
The present invention relates to gas gathering and transportation fields, and in particular to one kind is from high sulfur Gas Fields gathering system solid deposits
The method for detaching sulphur.
Background technology
In high sulfur-containing natural gas gas field, elementary sulfur is dissolved in the form of polysulfide in sulfur-containing gas, works as gas well
When exploitation, since temperature and pressure reduces, the amount of dissolving elementary sulfur can also be reduced in gas, and oversaturated sulphur will collect defeated system
It is precipitated, and then deposits in system.Meanwhile the defeated system production fortune of the silt particle that is carried out from shaft bottom of raw natural gas, hydro carbons sum aggregate
Corrosion inhibiter, hydrate inhibitor, the corrosion product etc. that row is added in the process are mixed in deposit, constitute high sulfur-containing natural gas
The complicated composition of gathering system solid deposits.
Currently, since high sulfur-containing natural gas gathering system solid deposits are difficult to efficiently separate recycling, usually according to solid
The process of body waste and Solid state fermentation is disposed, and burial is handled after solid deposits are burned, or is burned
It is used afterwards as the added material of cement.Environmental pollution is not only resulted in using the method for burning disposal, in synchronous deposits
Effective ingredient can not efficiently use.
In recent years, occur carrying out desulfurization process using biotechnology, i.e., it, will be useless containing sulphur by high-temperature oxidation
Admittedly generating sulfur dioxide or sulfur trioxide, lye sulfur dioxide absorption and sulfur trioxide is used to generate sulphite or sulfuric acid later
Salt, then by biological bacterium by biotransformation method be the sulphur that can be used as fertilizer by sulphite or sulfate conversion.
Use biological method can be with high efficiente callback sulphur, but cost is excessively high, complex process, limits its application, at present bioanalysis master
It is used for the removing of hydrogen sulfide in gas.
In addition, carry out sulphur recovery also by physico-chemical process, i.e., it is useless to sulfur-bearing to use high temperature admittedly in reaction kettle
Solid deposits are warming up to 400 DEG C or more by the mode of evaporation, and the sulphur distillation in giving up admittedly is the discharge of sulphur steam, and other useless
Admittedly staying in reaction kettle, then sulphur steam is recycled by condensation method, the sulfur purity of this method recycling is higher, but locates
Reason process is complicated, and cost is higher, and not disposable a large amount of sulfur-bearing is useless solid.
Therefore, relatively low, the simple for process sulfur recovery method of research cost, for being generated from high sulfur Gas Fields gathering system
A large amount of solid deposits in separation sulphur have important engineering significance.
Invention content
The purpose of the present invention is provide a kind of two-stage treatment for problems of the prior art and detach the side of sulphur
Method reduces influence of the presence of high sulfur-containing natural gas gathering system solid waste to gathering system.
Technical solution provided by the invention is：
The method that sulphur is detached from high sulfur Gas Fields gathering system solid deposits, includes the following steps：
(1) high sulfur Gas Fields gathering system solid deposits are placed in dryer or drying box, heat preservation a period of time goes
Moisture removal, methanol, corrosion inhibiter impurity obtain dry solid deposits A；
(2) the drying solid deposit A grind into powder that will be obtained in step (1) obtains powdery deposits B；
(3) configuration quality percentage is 80%~85% liquor zinci chloridi C in 60 DEG C~70 DEG C of water, and nitre is added
Acid or hydrochloride adjusted solution pH value；
(4) it in the liquor zinci chloridi C for preparing the solid deposits powder B merging steps (3) obtained in step (2), adopts
1 minute~10 minutes are stirred with 10 revs/min~1000 revs/min of speed, later with magnetic stirring apparatus or mechanical agitator
1 hour~3 hours are stood, stratified mixture D is obtained；
(5) liquid distributing device is used, the floating material in step (4) above stratified mixture D is taken out, obtains diatomite, sulphur
The mixture E of sulphur and a small amount of liquor zinci chloridi；
(6) configuration quality percentage is 55%~63% liquor zinci chloridi F in 15 DEG C~30 DEG C of water, and nitre is added
Acid or hydrochloride adjusted solution pH value；
(7) in the liquor zinci chloridi F for preparing the mixture E merging step (6) obtained in step (5), magnetic agitation is used
Device or mechanical agitator are stirred 1 minute~10 minutes with 10 revs/min~1000 revs/min of speed, stand 1 hour later~
3 hours, obtain stratified mixture G；
(8) liquid distributing device is used, the sediment below the stratified mixture G that step (7) is obtained takes out, and by sediment
It is dried at 60 DEG C~100 DEG C, that is, obtains the sulphur in high sulfur Gas Fields gathering system solid deposits.
Specifically, the high sulfur Gas Fields gathering system solid deposits main ingredient mass percent is：Sulphur contains
Amount 65%~80%, silicate content 5%~10%, sulphates content 1%~5%, diatomite content 1%~3%, methanol contains
Amount 1%~2%, Imidazoline corrosion inhibitor content 1%~2%, water content 1%~10%.
Specifically, dryer or drying box temperature are set as 60 DEG C~100 DEG C in the step (1), soaking time is more than
Equal to 5 hours.
Specifically, the powdery deposits B obtained in the step (2) can all pass through the sieve of 200 mesh.
Specifically, the pH value range for the liquor zinci chloridi C that the step (3) obtains is 3.5~4.5.
Specifically, the pH value range in liquor zinci chloridi F that the step (6) obtains is 3.5~4.5.
The method provided by the present invention that sulphur is detached from high sulfur Gas Fields gathering system solid deposits uses two level
Separating technology isolates the light components such as sulphur and the diatomite in high sulfur Gas Fields gathering system solid deposits, later first
Sulphur is isolated from the sulphur and diatomite separated again, lower can realize high sulfur Gas Fields collection in the case that consuming energy
The recycling of sulphur in defeated system solid deposits can be widely used in useless solid waste Slag treatment field of the oil gas field containing solid sulfur.
Description of the drawings
Fig. 1 is specific implementation mode 1 to the XRD before the progress sulphur separation of high sulfur Gas Fields gathering system solid deposits
Collection of illustrative plates；
Fig. 2 is separation after specific implementation mode 1 carries out sulphur separation to high sulfur Gas Fields gathering system solid deposits
The XRD spectrum of the sulphur gone out.
Specific implementation mode
Specific implementation mode 1
High sulfur Gas Fields gathering system solid deposits main ingredient mass percent is sulfur content 65%~80%, silicon
Phosphate content 5%~10%, sulphates content 1%~5%, diatomite content 1%~3%, methanol content 1%~2%, imidazoles
Quinoline type inhibition agent content 1%~2%, water content 1%~10%.
The method that sulphur is detached from high sulfur Gas Fields gathering system solid deposits, includes the following steps：
(1) 50g deposits are taken out of high sulfur Gas Fields gas collection yard metering separator, deposit is placed in air dry oven
Interior, air dry oven temperature is set in 80 DEG C, and heat preservation is taken out after 6 hours；
(2) by the drying solid deposit ball mill grinding obtained in step (1) at powder, with the sieve mistake of 200 mesh
Filter；
(3) the drying solid powder that will be obtained in step (2), using X-ray diffractometer analysed for powder object phase, it can be seen that
There is (as shown in Figure 1) containing calcium silicates, sodium metasilicate, diatomite and sulphur S8 phases in powder.
(4) configuration quality percentage is 80% liquor zinci chloridi in 70 DEG C of water, and nitric acid adjustment pH value of solution is added
Value is 4.0；
(5) it in the liquor zinci chloridi for preparing the solid deposits powder merging step (4) obtained in step (2), uses
Magnetic stirring apparatus is stirred 5 minutes with 100 revs/min of speed, is stood 1 hour later, is obtained stratified mixture；
(6) use glass liquid distribution funnel, by below step (5) stratified mixture deposit and solution be discharged, in acquisition
The diatomite of side, the mixture of sulphur and a small amount of liquor zinci chloridi；
(7) configuration quality percentage is 60% liquor zinci chloridi in 25 DEG C of water, and nitric acid adjustment pH value of solution is added
Value is 4；
(8) in the liquor zinci chloridi for preparing the mixture merging step (7) obtained in step (6), magnetic stirring apparatus is used
It is stirred 5 minutes with 100 revs/min of speed, stands 2 hours later, obtain stratified mixture：Sulphur is deposited in solution bottom,
Diatomite swims in superjacent；
(9) separatory funnel is used, the sediment below step (8) is taken out, that is, obtains the sulphur isolated；
(10) sulphur for obtaining step (9) is placed in 3 hours dry in 80 DEG C of air dry oven temperature, that is, is obtained from solid
The drying solid sulphur isolated in body deposit.
(11) the drying solid sulphur grind into powder that will be obtained in step (10), using X-ray diffractometer analysed for powder
Object phase, it can be seen that sulphur in powder and there is (as shown in Figure 2) with S8 phases.
Specific implementation mode 2
The operation of following steps unlike specific implementation mode 1：
(1) 50g deposits are taken out of high sulfur Gas Fields gas collection yard metering separator, deposit is placed in air dry oven
Interior, air dry oven temperature is set in 60 DEG C, and heat preservation is taken out after 8 hours；
(4) configuration quality percentage is 82% liquor zinci chloridi in 60 DEG C of water, and nitric acid adjustment pH value of solution is added
Value is 3.5；
(7) configuration quality percentage is 55% liquor zinci chloridi in 15 DEG C of water, and nitric acid adjustment pH value of solution is added
Value is 4；
Specific implementation mode 3
The operation of following steps unlike specific implementation mode 1：
(1) 50g deposits are taken out of high sulfur Gas Fields gas collection yard metering separator, deposit is placed in air dry oven
Interior, air dry oven temperature is set in 60 DEG C, and heat preservation is taken out after 8 hours；
(4) configuration quality percentage is 85% liquor zinci chloridi in 65 DEG C of water, and nitric acid adjustment pH value of solution is added
Value is 3.5；
(7) configuration quality percentage is 63% liquor zinci chloridi in 30 DEG C of water, and nitric acid adjustment pH value of solution is added
Value is 4；
Finally it should be noted that:The above embodiments are merely illustrative of the technical scheme of the present invention and are not intended to be limiting thereof；To the greatest extent
The present invention is described in detail with reference to preferred embodiments for pipe, those of ordinary skills in the art should understand that：Still
It can modify to the specific implementation mode of the present invention or equivalent replacement is carried out to some technical characteristics；Without departing from this hair
The spirit of bright technical solution should all cover within the scope of the technical scheme claimed by the invention.
Claims (6)
1. the method for detaching sulphur from high sulfur Gas Fields gathering system solid deposits, which is characterized in that include the following steps：
(1) high sulfur Gas Fields gathering system solid deposits are placed in dryer or drying box, heat preservation a period of time goes to remove water
Divide, methanol, corrosion inhibiter impurity, obtains dry solid deposits A；
(2) the drying solid deposit A grind into powder that will be obtained in step (1) obtains powdery deposits B；
(3) in 60 DEG C~70 DEG C of water configuration quality percentage be 80%~85% liquor zinci chloridi C, and be added nitric acid or
Hydrochloride adjusted solution pH value；
(4) in the liquor zinci chloridi C for preparing the solid deposits powder B merging steps (3) obtained in step (2), using magnetic
Power blender or mechanical agitator are stirred 1 minute~10 minutes with 10 revs/min~1000 revs/min of speed, stand 1 later
Hour~3 hours, obtain stratified mixture D；
(5) use liquid distributing device, floating material above stratified mixture D in step (4) taken out, obtain diatomite, sulphur with
The mixture E of a small amount of liquor zinci chloridi；
(6) in 15 DEG C~30 DEG C of water configuration quality percentage be 55%~63% liquor zinci chloridi F, and be added nitric acid or
Hydrochloride adjusted solution pH value；
(7) in the liquor zinci chloridi F for preparing the mixture E merging step (6) obtained in step (5), with magnetic stirring apparatus or
Mechanical agitator is stirred 1 minute~10 minutes with 10 revs/min~1000 revs/min of speed, and it is small to stand 1 hour~3 later
When, obtain stratified mixture G；
(8) liquid distributing device is used, the sediment below the stratified mixture G that step (7) is obtained takes out, and by sediment 60
DEG C~100 DEG C at dry, that is, obtain the sulphur in high sulfur Gas Fields gathering system solid deposits.
2. the method for detaching sulphur from high sulfur Gas Fields gathering system solid deposits according to claim 1, feature
It is, the high sulfur Gas Fields gathering system solid deposits main ingredient mass percent is：Sulfur content 65%~
80%, silicate content 5%~10%, sulphates content 1%~5%, diatomite content 1%~3%, methanol content 1%~
2%, Imidazoline corrosion inhibitor content 1%~2%, water content 1%~10%.
3. the method for detaching sulphur from high sulfur Gas Fields gathering system solid deposits according to claim 1, feature
It is, dryer or drying box temperature are set as 60 DEG C~100 DEG C in the step (1), and soaking time is more than or equal to 5 hours.
4. the method for detaching sulphur from high sulfur Gas Fields gathering system solid deposits according to claim 1, feature
It is, the powdery deposits B obtained in the step (2) can all pass through the sieve of 200 mesh.
5. the method for detaching sulphur from high sulfur Gas Fields gathering system solid deposits according to claim 1, feature
It is, the pH value range for the liquor zinci chloridi C that the step (3) obtains is 3.5~4.5.
6. the method for detaching sulphur from high sulfur Gas Fields gathering system solid deposits according to claim 1, feature
It is, the pH value range in liquor zinci chloridi F that the step (6) obtains is 3.5~4.5.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105000745A (en) * | 2015-09-02 | 2015-10-28 | 中国石油化工股份有限公司 | Sulfur gas field produced water treatment system |
| CN105174581A (en) * | 2015-09-02 | 2015-12-23 | 中国石油化工股份有限公司 | Sulfur-containing gas field produced water treatment process |
| CN105523596A (en) * | 2014-09-30 | 2016-04-27 | 李向东 | Gas field sewage harmless treatment method |
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2016
- 2016-08-31 CN CN201610775168.9A patent/CN106185833B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105523596A (en) * | 2014-09-30 | 2016-04-27 | 李向东 | Gas field sewage harmless treatment method |
| CN105000745A (en) * | 2015-09-02 | 2015-10-28 | 中国石油化工股份有限公司 | Sulfur gas field produced water treatment system |
| CN105174581A (en) * | 2015-09-02 | 2015-12-23 | 中国石油化工股份有限公司 | Sulfur-containing gas field produced water treatment process |
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