CN106744703A - A kind of compound eluent of coking sulphur cream and preparation method thereof - Google Patents
A kind of compound eluent of coking sulphur cream and preparation method thereof Download PDFInfo
- Publication number
- CN106744703A CN106744703A CN201611006056.3A CN201611006056A CN106744703A CN 106744703 A CN106744703 A CN 106744703A CN 201611006056 A CN201611006056 A CN 201611006056A CN 106744703 A CN106744703 A CN 106744703A
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- CN
- China
- Prior art keywords
- sulphur
- sulphur cream
- cream
- eluent
- quinoline
- 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.)
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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
- C01B17/033—Recovery of sulfur from material containing elemental sulfur, e.g. luxmasses or sulfur containing ores; Purification of the recovered sulfur using a liquid extractant
Abstract
The invention discloses a kind of compound eluent of coking sulphur cream and preparation method thereof, the eluent is made up of ammoniacal liquor, quinoline, dodecyl phenenyl sulfate, MEA, ethylenediamine and organic phosphoric acid；The preparation method is by ammoniacal liquor, MEA, ethylenediamine and organic phosphate, mixing, heating is stirred at room temperature and obtains basic solution, dodecyl phenenyl sulfate is added in basic solution afterwards, it is stirred simultaneously, until after dodecyl phenenyl sulfate is completely dissolved, quinoline is added again, until the quinoline for adding fully dissolves, that is, obtains the compound eluent of sulphur cream.The compound eluent items stable in physicochemical property that the present invention is developed, it is with low cost, the impurity such as ammonium thiocyanate, ATS (Ammonium thiosulphate), ammonium sulfate, ferrous sulfate, phenols and the tar organic matter that can effectively go in sulphur removal cream, on the premise of a large amount of inflammable and explosive organic solvents are not introduced into, the efficient purification of sulphur cream is realized, the pollution problem of sulphur cream is solved.
Description
Technical field
The present invention relates to a kind of eluent and preparation method thereof, the compound eluent of particularly a kind of coking sulphur cream purification and
Its preparation method.
Background technology
Coal chemical enterprise sulfur content ＞ 50% in the byproduct sulphur cream obtained using ammonia process Wet-type oxidation sweetening technique, is contained
There are the organic matters such as the desulfuration byproducts such as substantial amounts of moisture, rhodanate and thiosulfate, phenols and tar and desulfurization catalyst
The impurity such as agent, are a kind of difficult utilization, heavy-polluted industrial solid castoff.But the main component sulphur in sulphur cream agricultural,
Each fields such as medicine, rubber, building, gunpowder, match, wine brewing and sugaring are widely used, and effective recycling is burnt
Changing sulphur cream will be significant.
Conventional method generally uses fusion method and carries out purification processes to sulphur cream, and the method is the temperature model at 125 DEG C ~ 158 DEG C
In enclosing, by sulphur cream by obtaining sulphur after fusing-filter progress, the purpose of sulphur purification is reached.Although can in melting process
Sulphur is effectively separated with the difference of doctor solution density with using molten sulfur, but the sulphur color hair for obtaining by this method
Black, purity is relatively low, and use value is low, at the same also there are problems that highly energy-consuming, heavily contaminated and.Therefore most coal chemical enterprises
Directly sulphur cream returned enterprise can be given to undersell using sulphur cream as product, but be limited to the tired of the downstream industries such as sulfuric acid and chemical fertilizer
Soft, the situation of the long-term low level operation of the price of sulphur cannot change in a short time, thus coal chemical enterprise often need 20 ~ 40 yuan of payment/
Returned enterprise of the price of ton even more high to sulphur cream.The enterprise that part sulphur cream is reclaimed realizes the purification of sulphur cream by evaporating method,
But due to organic matter and desulfurization catalysts such as desulfuration byproduct, phenols and the tar such as the rhodanate and thiosulfate in sulphur cream
The impurity such as agent can decompose the generation pollutant such as hydrogen sulfide and ammonia in sulphur cream gasification, and such enterprise it is general without
Treatment is directly discharged into air, there is serious problem of environmental pollution, therefore prohibits the use of the method to carry out sulphur cream by environmental administration
Treatment, thus sulphur cream also just often sinks into unsalable awkward situation.In order to maintain normal production, there is coal chemical enterprise even directly to make sulphur cream
For discarded object is filled, the wasting of resources is so not only caused, severe contamination environment also threatens the safety of workman and the periphery masses and is good for
Health.
There is part researcher to do correlative study to the sulphur in purification sulphur cream at present, Niu Yanxia is carried out with toluene to sulphur cream
Leaching, by soxhlet type apparatus, has obtained the sulphur that purity is more than 95%；Publication No. CN104192811A discloses one
Plant sulphur cream is leached using carbon disulfide, although organic solvent soaking extraction method can obtain high-purity sulphur, but leaching process draws
Enter a large amount of organic solvents, there is the safety problems such as inflammable and explosive and toxicity is big, and leaching agent price is far above Sulfur price,
Therefore it is not applied in the treatment of coking sulphur cream.The patent of Yang Xiaojin applications, the patent of Publication No. CN204224257U
The device of Recovered sulphur, is processed dehydrated sulfur cream, using nitric acid using nitric acid oxidation method in disclosing a kind of foam from sulphur
Oxidisability by the SCN in sulphur cream-、S2O3 2-Sulphur simple substance is oxidized to Deng material, while removing organic impurities therein, sulphur cream is processed
Effect is significant.But the method reaction is violent, there is substantial amounts of nitrogen dioxide to produce in course of reaction, there is high energy consumption and heavy-polluted
Problem.The patent of Li Tao et al. applications, the patent of Publication No. CN106006569A discloses a kind of ammonia process wet type desulfurizing technique
The purifying technique of accessory substance sulphur cream, employs the technique that the technology such as elution and melting is combined, and solves what the melting of sulphur cream was obtained
The problem that sulphur blacks, purity is low, but the formula and preparation method to eluent are not explained in detail.
The content of the invention
The purpose of the present invention is to coordinate " a kind of purifying technique of ammonia process wet type desulfurizing process byproducts sulphur cream " and provide
A kind of compound eluent of coking sulphur cream and preparation method thereof.The compound eluent items stable in physicochemical property, with low cost, energy
The impurity such as ammonium thiocyanate, ATS (Ammonium thiosulphate), ammonium sulfate, ferrous sulfate, phenols and the tar organic matter for effectively going in sulphur removal cream,
On the premise of being not introduced into a large amount of inflammable and explosive organic solvents, the efficient purification of sulphur cream is realized, solve the pollution problem of sulphur cream.
To achieve the above object, this invention takes following technical scheme.
A kind of compound eluent of coking sulphur cream, it is characterised in that：The composition and its weight portion of the compound eluent are such as
Under：
10% ~ 30% 75 ~ 90 parts of ammoniacal liquor
1 ~ 5 part of quinoline
2 ~ 7 parts of dodecyl phenenyl sulfate
1 ~ 6 part of MEA
2 ~ 3 parts of ethylenediamine
1 ~ 5 part of organic phosphate
Present invention also offers a kind of preparation method of the compound eluent for above-mentioned coking sulphur cream, the preparation method is
It follow these steps to what is carried out：
（1）By 10% ~ 30% ammoniacal liquor, MEA, ethylenediamine and organic phosphate, it is thoroughly mixed at room temperature, then will
Said mixture is heated to 60 DEG C ~ 80 DEG C, obtains basic solution；
（2）By 2 ~ 7 parts of dodecyl phenenyl sulfate be added to it is described obtain basic solution, be maintained at 70 DEG C ~ 90 DEG C simultaneously
It is stirred, until after dodecyl phenenyl sulfate is completely dissolved, then 1 ~ 5 part of quinoline is uniformly divided into 2-5 additions, until
The quinoline of addition fully dissolves, that is, obtain the compound eluent of sulphur cream, and use at 70 DEG C ~ 90 DEG C.
Basic solution therein is that by 10% ~ 30% 75 parts ~ 90 parts of ammoniacal liquor, 1 ~ 6 part of MEA, 2 ~ 3 parts of ethylenediamine, have
1 ~ 5 part of mixed preparing of machine phosphate is formed.
Implement compound eluent of a kind of coking sulphur cream that the invention described above is provided and preparation method thereof, be in existing skill
On the basis of art, coordinate " a kind of purifying technique of ammonia process wet type desulfurizing process byproducts sulphur cream " and propose, with prior art
Compare, have the following advantages and good effect.
The present invention is obtained on the premise of a large amount of inflammable and explosive organic solvents are not introduced into for ammonia process wet type desulfurizing technique
Urged containing the organic matters such as desulfuration byproduct, phenols and the tar such as rhodanate and thiosulfate and desulfurization in byproduct sulphur cream
The impurity of agent, by the ammoniacal liquor in the compound eluent of sulphur cream, MEA, ethylenediamine, organic phosphate can be by rhodanate
With water-dissolving phase material and the Fe such as thiosulfate2+Deng heavy metals removal, the detergent alkylate in the compound eluent of next sulphur cream
Sodium sulfonate and quinoline respectively can remove organic substance phenols and tar, solve the pollution problem of sulphur cream, realize sulphur cream
Simple economy is purified.
Brief description of the drawings
Fig. 1 be the embodiment of the present invention elution before and after ion concentration table figure.
Fig. 2 is the FT-IR contrast curves of the embodiment of the present invention.
Fig. 3 is the XRF comparison diagrams of the embodiment of the present invention.
Specific embodiment
Specific embodiment of the invention is made further instructions below.
Embodiment 1
Step 1：Prepare raw material by following weight：15% ammoniacal liquor 80g, quinoline 1g, dodecyl phenenyl sulfate 6g, MEA
5g, ethylenediamine 3g, organic phosphate 5g.
Step 2：15% ammoniacal liquor 80g, MEA 5g, ethylenediamine 3g, organic phosphate 5g are sufficiently stirred for mixing at room temperature
Close, then said mixture is heated to 60 DEG C, obtain basic solution.
Step 3：6g dodecyl phenenyl sulfates are added in the basic solution of step 1,70 DEG C is maintained the temperature at similarly hereinafter
When be stirred, until after dodecyl phenenyl sulfate is completely dissolved, 1g quinoline is uniformly divided into repeatedly addition, until adding
Quinoline fully dissolve, that is, obtain the compound eluent of sulphur cream, and use at a temperature of being maintained at 70 DEG C.
Product after being eluted by coking sulphur cream and through composite detergent carries out ion measurement, and its measurement result sees attached list Fig. 1.
Knowable to subordinate list Fig. 1, after coking sulphur cream is processed through compound eluent, sulfur content substantially rises, SCN-、S2O3 2-、
SO4 2-、Fe2+/Fe3+Removed Deng water-dissolving phase material, illustrated the eluent to ammonium thiocyanate, ATS (Ammonium thiosulphate), ammonium sulfate, sulfuric acid
The water-solubility impurities such as ferrous iron have preferable removal effect.
FT-IR and XRF is respectively adopted carries out table to the organic matter and tenor situation of change in the sulphur cream before and after elution
Levy analysis.Accompanying drawing 2 is elution sample and the FT-IR contrast curves of sulphur cream former state, and accompanying drawing 3 is elution sample and the XRF of sulphur cream former state
Comparison diagram.
Be can be seen that after coking sulphur cream processes through eluent from the FT-IR contrast curves of accompanying drawing 2, aromatic hydrocarbons, phenols etc.
Organic matter has obtained effective removal, in 2053cm-1Stretching vibration peak, the 1400cm of neighbouring C ≡ N-1Neighbouring aromatic hydrocarbons C=C
The stretching vibration peak of key, 615cm-1The vibration peak of neighbouring C-Cl keys has disappeared, and illustrates the eluent to phenols and tar etc.
Organic phase impurity has a preferable removal effect.
After can be seen that coking sulphur cream through compound eluent treatment from the XRF of accompanying drawing 3 contrast block diagrams, S constituent contents are bright
Aobvious to rise, the element such as Fe, Br, Cl, P is removed substantially.Illustrate that the eluent there are the impurity such as the class salt such as inorganic metal preferably to go
Except effect.
Claims (3)
1. a kind of compound eluent of coking sulphur cream, it is characterised in that：The composition and its weight portion of the compound eluent are as follows：
10% ~ 30% 75 ~ 90 parts of ammoniacal liquor；
1 ~ 5 part of quinoline；
2 ~ 7 parts of dodecyl phenenyl sulfate；
1 ~ 6 part of MEA；
2 ~ 3 parts of ethylenediamine；
1 ~ 5 part of organic phosphate.
2. the preparation method of a kind of compound eluent for coking sulphur cream as claimed in claim 1, the preparation method is
It follow these steps to what is carried out：
（1）By 10% ~ 30% ammoniacal liquor, MEA, ethylenediamine and organic phosphate, it is thoroughly mixed at room temperature, then will
Said mixture is heated to 60 DEG C ~ 80 DEG C, obtains basic solution；
（2）By 2 ~ 7 parts of dodecyl phenenyl sulfate be added to it is described obtain basic solution, be maintained at 70 DEG C ~ 90 DEG C simultaneously
It is stirred, until after dodecyl phenenyl sulfate is completely dissolved, then 1 ~ 5 part of quinoline is uniformly divided into 2-5 additions, until
The quinoline of addition fully dissolves, that is, obtain the compound eluent of sulphur cream, and use at 70 DEG C ~ 90 DEG C.
3. preparation method as claimed in claim 2, the basic solution is by 10% ~ 30% 75 parts of ammoniacal liquor ~ 90 parts, monoethanol
1 ~ 6 part of amine, 2 ~ 3 parts of ethylenediamine, 1 ~ 5 part of mixed preparing of organic phosphate are formed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611006056.3A CN106744703A (en) | 2016-11-16 | 2016-11-16 | A kind of compound eluent of coking sulphur cream and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611006056.3A CN106744703A (en) | 2016-11-16 | 2016-11-16 | A kind of compound eluent of coking sulphur cream and preparation method thereof |
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| CN106744703A true CN106744703A (en) | 2017-05-31 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114477098A (en) * | 2021-12-17 | 2022-05-13 | 湖南道安环保科技有限公司 | Purification process of byproduct sulfur in HPF (high pressure fluidized bed) desulfurization |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101198416A (en) * | 2005-04-15 | 2008-06-11 | 高级技术材料公司 | Formulations for cleaning ion-implanted photoresist layers from microelectronic devices |
| CN106006569A (en) * | 2016-05-16 | 2016-10-12 | 太原理工大学 | Purification process for by-product sulfur paste of ammonia-method wet type desulfurization process |
-
2016
- 2016-11-16 CN CN201611006056.3A patent/CN106744703A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101198416A (en) * | 2005-04-15 | 2008-06-11 | 高级技术材料公司 | Formulations for cleaning ion-implanted photoresist layers from microelectronic devices |
| CN106006569A (en) * | 2016-05-16 | 2016-10-12 | 太原理工大学 | Purification process for by-product sulfur paste of ammonia-method wet type desulfurization process |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114477098A (en) * | 2021-12-17 | 2022-05-13 | 湖南道安环保科技有限公司 | Purification process of byproduct sulfur in HPF (high pressure fluidized bed) desulfurization |
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Application publication date: 20170531 |
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