CN105399178A - Agglomeration solution and removing method - Google Patents
Agglomeration solution and removing method Download PDFInfo
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- CN105399178A CN105399178A CN201510896295.XA CN201510896295A CN105399178A CN 105399178 A CN105399178 A CN 105399178A CN 201510896295 A CN201510896295 A CN 201510896295A CN 105399178 A CN105399178 A CN 105399178A
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Abstract
The embodiment of the invention provides an agglomeration solution and a removing method, and relates to the field of water treatment. By means of the agglomeration solution, the adhesion of sulfate produced by materials during supercritical water oxidation treatment to the inner wall of a reaction device can be effectively reduced, corrosion to the device is effectively prevented, and sulfate is prevented from blocking the narrow space of the reaction device. The agglomeration solution comprises a nucleating agent, an adsorption agent and a crosslinking agent, wherein the nucleating agent is mainly prepared from calcium hydroxide and used for adsorbing sulfate produced during supercritical water oxidation treatment to form compound particles, the adsorption agent is mainly prepared from silicon oxide and used for adsorbing compound particles, and the crosslinking agent is mainly prepared from aluminum oxide and used for forming compound aggregate together with the adsorption agent adsorbing the compound particles. The embodiment of the invention is used for preparing the agglomeration solution.
Description
Technical field
The present invention relates to water treatment field, particularly relate to a kind of agglomerator and minimizing technology.
Background technology
Supercritical water, refers to when air pressure and temperature reach certain value, Yin Gaowen and the density of the water expanded and water time just in time identical by the density of water vapour compressed because of high pressure.Now, the liquids and gases state of water is as broad as long, blends completely together, becomes a kind of liquid presenting high pressure-temperature state newly.Supercritical water has strong reactive behavior, and the material of the process of needs is put into supercritical water, is filled with oxygen and hydrogen peroxide, and this material will oxidized and hydrolysis.Due to this diverse with the normal temperature and pressure water physicochemical property that supercritical water has, it all has wide practical use in the many-side such as environmental protection, gasification.
Supercritical water oxidation method treatment technology utilizes supercritical water as medium, under high-temperature and high-pressure conditions, organism oxygen contained in waste water or sewage resolved into the simply nontoxic micromolecular compound such as water, carbonic acid gas.Because supercritical water oxidation method treatment technology almost reaches 100% to organism clearance rate contained in waste water or sewage, and be fully oxidized at full closeding state organism, non-secondary pollution, therefore, technique is subject to people's attention day by day.
Time more than 450 DEG C, the solubleness of inorganic salt (mainly comprising vitriol) in supercritical water contained in waste water or sewage is very little.When reaching the hypersaturated state of inorganic salt, when the condition such as the temperature in supercritical reaction device, pressure, flow field changes, inorganic salt can be separated out with solid form and be attached on equipment inner wall, thus cause corrosion gradually to equipment.Inorganic salt concentration contained in a lot of waste water or sewage is very high, utilizes during supercritical water oxidation method process and can cause serious corrosion to the material inside of conversion unit.In addition, organic molecule chain contained in some waste water or sewage exists S (sulphur) atom of organic, the vitriol of highest oxidation state can be transformed into after organism generation oxidizing reaction, exacerbate the corrosion to conversion unit.In addition, the adhesion of a large amount of vitriol, also can cause the blocking of conversion unit stenosis, affect reaction efficiency.
Therefore, the difficult point that a large amount of solid-state vitriol that material separates out in supercritical water oxidation method becomes supercritical water treatment technology how is removed.
Summary of the invention
Embodiments of the invention provide a kind of agglomerator and minimizing technology, adopt this agglomerator effectively to reduce vitriol that material produces in supercritical water oxidation process is to the adhesion of conversion unit inwall, effectively prevent equipment corrosion, avoid vitriol to be blocked in the stenosis of conversion unit.For achieving the above object, embodiments of the invention adopt following technical scheme:
On the one hand, embodiments provide a kind of agglomerator, described agglomerator comprises: nucleator, sorbent material and linking agent; Wherein, described nucleator is formed primarily of calcium hydroxide, for adsorbing the vitriol that material produces in supercritical water oxidation process, to form compound particle; Described sorbent material is formed primarily of the oxide compound of silicon, for adsorbing described compound particle; Described linking agent is formed primarily of aluminum oxide, for forming composite aggregate with the described sorbent material being adsorbed with described compound particle.
Optionally, the quality of described calcium hydroxide accounts for the ratio span of described agglomerator total mass is 12.7% ~ 15.5%; The ratio span that the quality of described aluminum oxide accounts for described agglomerator total mass is 1.8% ~ 2.5%; The ratio span that the quality of the oxide compound of described silicon accounts for described agglomerator total mass is 78.0% ~ 82.0%.
Preferably, the quality of described calcium hydroxide accounts for the ratio span of described agglomerator total mass is 13.0% ~ 15.1%; The ratio span that the quality of the oxide compound of described silicon accounts for described agglomerator total mass is 78.3% ~ 81.6%.
Optionally, the particle diameter span of the oxide compound of described calcium hydroxide, described aluminum oxide and described silicon is 60 ~ 100 orders.
Optionally, the oxide compound of described silicon comprises: SiO
2, at least one in SiO.
On the other hand, the embodiment of the present invention additionally provides a kind of minimizing technology for removing the vitriol that material produces in supercritical water oxidation process, and described minimizing technology comprises: in supercritical reaction device, add material and agglomerator carries out supercritical water oxidation process; Described agglomerator is the agglomerator described in above-mentioned any one; Remove the composite aggregate being deposited in described supercritical reaction device bottom.
Optionally, the add-on of described agglomerator is 2.8 ~ 3.1 times of the element sulphur quality that described material comprises.
Optionally, the particle diameter span of the described composite aggregate of formation is 1 ~ 6mm.
Optionally, described removal is deposited in the composite aggregate of described supercritical reaction device bottom, specifically comprise: the temperature reducing described supercritical reaction device bottom, make the vitriol in described composite aggregate be dissolved in the aqueous solution, the insoluble substance including the insoluble compound in described composite aggregate is gathered in the bottom of described supercritical reaction device bottom; The bottom giving off described supercritical reaction device bottom is dissolved with the aqueous solution of described vitriol and the described insoluble substance of gathering.
Preferably, the temperature of described supercritical reaction device bottom is reduced to and is more than or equal to room temperature and is less than 100 DEG C.
Based on this, by the above-mentioned agglomerator that the embodiment of the present invention provides, oxide compound primarily of the calcium hydroxide as nucleator, the silicon as sorbent material and the aluminum oxide as linking agent are formed, the vitriol eutectoid of the highest oxidation state that can be formed at supercritical conditions with the S element in material, form the less composite aggregate of adhesivity and be deposited in the bottom of supercritical reaction device thus be removed, reduce vitriol separate out in supercritical reaction and then be attached to the degree on equipment inner wall, thus decrease corrosion is caused to equipment.And the vitriol avoiding precipitation is blocked in the stenosis of reactor and impacts supercritical reaction.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
A kind of minimizing technology schematic flow sheet for removing the vitriol that material produces in supercritical water oxidation process that Fig. 1 provides for the embodiment of the present invention.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
It is pointed out that unless otherwise defined, all terms (comprising technology and scientific terminology) used in the embodiment of the present invention have the identical meanings jointly understood with those skilled in the art.It should also be understood that, those terms such as defined in usual dictionary should be interpreted as having the consistent implication of implication with them in the context of correlation technique, and do not apply idealized or extremely formal meaning explain, unless defined so clearly here.
Embodiments provide a kind of agglomerator, this agglomerator comprises: nucleator, sorbent material and linking agent; Wherein, nucleator is formed primarily of calcium hydroxide, for adsorbing the vitriol that material produces in supercritical water oxidation process, to form compound particle; Sorbent material is formed primarily of the oxide compound of silicon, for adsorbing above-mentioned compound particle; Linking agent is formed primarily of aluminum oxide, for forming composite aggregate with the above-mentioned sorbent material being adsorbed with compound particle.
It should be noted that, first, agglomerator primarily of nucleator, sorbent material and linking agent form, each composition effect and absorption principle as described below:
(1), the absorption of vitriol
Carry out in the process of supercritical reaction at material, the S element in the solid-state vitriol that calcium hydroxide can be separated out in supercritical water oxidation process with material combines, and forms the less calcium sulfate (CaSO of solubleness through oxidation
4) suspended substance, calcium hydroxide with this suspended substance for core, can make the vitriol in supercritical reaction system constantly adsorb thereon and grows up gradually for compound particle.The oxide compound of silicon can catch the compound particle of above-mentioned vitriol nucleation and growth process formation, and compound particle is reunited together further.And aluminum oxide (Al
2o
3) owing to there is close oxide lattice structure with the oxide compound of silicon, therefore, it is possible to form the composite oxides of reunion state further with the oxide compound of the silicon being adsorbed with above-claimed cpd particle, the composite aggregate that namely volume is larger.
Here, the vitriol that the S element in material is formed at supercritical conditions can with above-mentioned oxyhydroxide and oxide compound eutectoid, form that adhesivity is less, composite aggregate that volume is larger.
Wherein, the oxide compound of silicon can be such as SiO
2at least one in (silicon-dioxide), SiO (silicon monoxide), due to the SiO of amorphous state
2extensively be present in occurring in nature, raw material is easy to obtain, and the SiO of amorphous state
2springy texture and porous, quality are relatively light, adsorptivity is strong, more effectively can adsorb the compound particle that above-mentioned vitriol nucleation and growth process is formed, and therefore preferred further, the oxide compound of silicon is the SiO of amorphous state
2powder.
Sorbent material will be adsorbed after the compound particle of growing up is attached together by nucleator, the larger composite aggregate of volume is formed further with linking agent, be equivalent to reduce the area that in prior art, in supercritical reaction system, single vitriol exposes, reduce vitriol to separate out and then the degree that is attached on equipment inner wall, thus decrease corrosion is caused to equipment.
(2), the removal of vitriol
Because the larger quality of composite aggregate volume is also heavier, under gravity, the bottom of supercritical reaction device can be deposited to.Low temperature (this low temperature is generally and is more than or equal to room temperature and is less than 100 DEG C) is kept by making the bottom of supercritical reaction device, the vitriol in above-mentioned composite aggregate can be made to be dissolved in gradually in the aqueous solution, insoluble substance (what to include in insoluble compound as each oxide component in agglomerator is formed and supercritical reaction other is reduced to the insoluble physical property compound of less than 100 DEG C when temperature) is gathered in the bottom of the bottom of supercritical reaction device with the form of dispersed (particle diameter is less than 0.4mm usually), can to release discharge from the opening end of bottom when reaching a certain amount of, thus eliminate the solid-state vitriol that material produces in supercritical water oxidation process.
Here, above-mentioned " room temperature ", also referred to as normal temperature or general temperature, as a rule, room temperature has the definition of 3 kinds of scopes, that is: (1), 23 DEG C ± 2 DEG C; (2), 25 DEG C ± 5 DEG C; (3), 20 DEG C ± 5 DEG C.
The second, in above-mentioned agglomerator, in massfraction, each component ratio of agglomerator is preferably as follows: the ratio span that the quality of calcium hydroxide accounts for agglomerator total mass is 12.7% ~ 15.5%; The ratio span that the quality of aluminum oxide accounts for agglomerator total mass is 1.8% ~ 2.5%; The ratio span that the quality of the oxide compound of silicon accounts for agglomerator total mass is 78.0% ~ 82.0%.
Above-mentioned each component further preferred ratio span is: the ratio span that the quality of calcium hydroxide accounts for described agglomerator total mass is 13.0% ~ 15.1%; The ratio span that the quality of the oxide compound of silicon accounts for described agglomerator total mass is 78.3% ~ 81.6%.Here, the ratio that the mass ratio due to aluminum oxide accounts for above-mentioned agglomerator total mass is less, so the ratio of place to aluminum oxide is optimized no longer further.
Here it is to be noted, because the amount of industrial treatment waste water, sewage is very large, usually calculate with tonnage, the purity of each component is difficult to reach the pure and above purity of accurate chemical analysis, each oxide compound may also have a certain proportion of crystal water, or is adsorbed with a certain amount of planar water and/or there is the invalid components such as other impurity.Therefore, each ratio is only to form the effective constituent of above-mentioned agglomerator above, namely the compound quality of the oxide compound of calcium hydroxide, aluminum oxide and silicon is basis, when each mass ratio sum of oxide compound of calcium hydroxide, aluminum oxide and silicon is less than 100%, remaining composition is then mainly water and/or other impurity.
Three, easily there is self when the particle diameter of each component compound is too small to reunite, and decrease and contact with the absorption of vitriol; When particle diameter is excessive, specific surface area is less, is also unfavorable for contacting with the absorption of vitriol.Therefore, the particle diameter of each component in agglomerator should in a suitable scope, and preferably, the particle diameter span of the oxide compound of calcium hydroxide, aluminum oxide and silicon is 60 ~ 100 orders (be 0.25 ~ 0.15mm corresponding to the millimeter mm order of magnitude).Further preferred, the particle diameter of each component oxide is all less than 80 orders (be 0.18mm corresponding to the millimeter mm order of magnitude).
Based on this, by the above-mentioned agglomerator that the embodiment of the present invention provides, oxide compound primarily of the calcium hydroxide as nucleator, the silicon as sorbent material and the aluminum oxide as linking agent are formed, the vitriol eutectoid that can be formed at supercritical conditions with the S element in material, form the less composite aggregate of adhesivity and be deposited in the bottom of supercritical reaction device thus be removed, reduce vitriol separate out in supercritical reaction and then be attached to the degree on equipment inner wall, thus decrease corrosion is caused to equipment.And the vitriol avoiding precipitation is blocked in the stenosis of reactor and impacts supercritical reaction.
On the basis of the above, the embodiment of the present invention additionally provides a kind of minimizing technology for removing the vitriol that material produces in supercritical water oxidation process, and this minimizing technology comprises:
S01, the agglomerator adding material and have above-mentioned each component in supercritical reaction device carry out supercritical water oxidation process;
S02, remove and be deposited in the composite aggregate of supercritical reaction device bottom.
For above-mentioned steps S01, because the S element in material is transformed into vitriol in supercritical reaction, in order to catch the vitriol that material is separated out at supercritical conditions, need a certain proportion of above-mentioned agglomerator of blending in material.The solid-state vitriol of precipitation can not be caught fully when considering that agglomerator add-on is very few, and catch vitriol limited in one's ability due to agglomerator, add-on too much also can cause the waste of agglomerator, therefore preferred, the additional proportion of agglomerator and material can be: the add-on of agglomerator is 2.8 ~ 3.1 times of the element sulphur quality that material comprises.That is, material often comprises 1gS element, adds the above-mentioned agglomerator of 2.8 ~ 3.1g.
Absorption through agglomerator is reunited, and the particle diameter span of the composite aggregate of formation is 1 ~ 6mm, is easy to be deposited to the bottom of supercritical reaction device under gravity to be removed further.
On the basis of the above, step S02 specifically comprises following sub-step:
The temperature of S21, reduction supercritical reaction device bottom, make the vitriol in composite aggregate be dissolved in the aqueous solution, the insoluble substance including the insoluble compound in above-mentioned composite aggregate is gathered in the bottom of supercritical reaction device bottom;
S22, the bottom giving off supercritical reaction device bottom are dissolved with the aqueous solution of vitriol and the insoluble substance of gathering.
It should be noted that, due to the composite aggregate particle size comparatively large (being generally 1 ~ 6mm) that gravitate is deposited in supercritical reaction device bottom, likely can some pipelines of clogging supercritical reaction device bottom if directly solid-state composite aggregate is given off from the opening part of supercritical reaction device bottom.Therefore, the embodiment of the present invention preferably adopts above-mentioned steps S21 and step S22 to remove the composite aggregate being deposited in supercritical reaction device bottom.
Temperature by supercritical reaction device bottom reduces and keeps low temperature (this low temperature is usually more than or equal to room temperature and is less than 100 DEG C), the vitriol be deposited in the composite aggregate of supercritical reaction device bottom is dissolved in the aqueous solution, and is gathered in the bottom of reactor lower part with the insoluble substance existed with dispersed (particle diameter is less than 0.4mm usually) form.From releasing discharge from the bottom open end of reactor lower part when reaching a certain amount of, thus eliminate the solid-state vitriol that material produces in supercritical water oxidation process.Here, what the insoluble compound existed with dispersed form to include in the insoluble compound and supercritical reaction that each oxide component in agglomerator formed other is reduced to the insoluble compound etc. of less than 100 DEG C when temperature of reaction.In above-mentioned process of releasing, while releasing, the water identical with the amount of releasing can passed into supercritical reaction device bottom, to keep the balance of W-response in supercritical reaction device.
Here, above-mentioned " room temperature ", also referred to as normal temperature or general temperature, as a rule, room temperature has the definition of 3 kinds of scopes, that is: (1), 23 DEG C ± 2 DEG C; (2), 25 DEG C ± 5 DEG C; (3), 20 DEG C ± 5 DEG C.
On the basis of the above, the embodiment of the present invention further provides 3 simultaneous tests, to verify the adsorbing and removing effect of above-mentioned agglomerator to vitriol further.
The reaction conditions choosing supercritical water oxidation process is: below pressure 23MPa, pH=6, containing 0.5% oxygen atmosphere.Use the material of sodium sulfate (using S element) as supercritical reaction of different concns, sulfate radical (SO in the solution of detection reaction device bottom after off-test
4 2-) concentration, be converted into S element quality, to calculate the decreasing ratio of vitriol.Wherein, in per kilogram material in S element and agglomerator each constituent mass following (unit is g):
Test one
| S | SiO 2 | Al 2O 3 | Ca(OH) 2 |
| 1.05 | 2.39 | 0.07 | 0.44 |
Wherein, the total mass of agglomerator is 2.96g, and the S element quality obtaining after testing reclaiming in reactor lower part solution is 0.96g, is 91.4% by calculating total removal efficiency of S.
Test two
| S | SiO 2 | Al 2O 3 | Ca(OH) 2 |
| 1.97 | 4.67 | 0.13 | 0.86 |
Wherein, the total mass of agglomerator is 5.87g, and the S element quality obtaining after testing reclaiming in reactor lower part solution is 1.89g, is 95.9% by calculating total removal efficiency of S.
Test three
| S | SiO 2 | Al 2O 3 | Ca(OH) 2 |
| 3.24 | 8.09 | 0.24 | 1.27 |
Wherein, the total mass of agglomerator is 9.98g, and the S element quality obtaining after testing reclaiming in reactor lower part solution is 2.93g, is 90.4% by calculating total removal efficiency of S.
As can be seen from above-mentioned test, the removal efficiency of vitriol, up to more than 90%, significantly reduces the adhesion to reactor wall when vitriol is separated out, and reduces the corrosion damage of vitriol attachment to reactor apparatus main body.
The above; be only the specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; change can be expected easily or replace, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of described claim.
Claims (10)
1. an agglomerator, is characterized in that, described agglomerator comprises: nucleator, sorbent material and linking agent;
Wherein, described nucleator is formed primarily of calcium hydroxide, for adsorbing the vitriol that material produces in supercritical water oxidation process, to form compound particle;
Described sorbent material is formed primarily of the oxide compound of silicon, for adsorbing described compound particle;
Described linking agent is formed primarily of aluminum oxide, for forming composite aggregate with the described sorbent material being adsorbed with described compound particle.
2. agglomerator according to claim 1, is characterized in that,
The ratio span that the quality of described calcium hydroxide accounts for described agglomerator total mass is 12.7% ~ 15.5%;
The ratio span that the quality of described aluminum oxide accounts for described agglomerator total mass is 1.8% ~ 2.5%;
The ratio span that the quality of the oxide compound of described silicon accounts for described agglomerator total mass is 78.0% ~ 82.0%.
3. agglomerator according to claim 2, is characterized in that,
The ratio span that the quality of described calcium hydroxide accounts for described agglomerator total mass is 13.0% ~ 15.1%;
The ratio span that the quality of the oxide compound of described silicon accounts for described agglomerator total mass is 78.3% ~ 81.6%.
4. agglomerator according to claim 1, is characterized in that, the particle diameter span of the oxide compound of described calcium hydroxide, described aluminum oxide and described silicon is 60 ~ 100 orders.
5. agglomerator according to claim 1, is characterized in that, the oxide compound of described silicon comprises: SiO
2, at least one in SiO.
6. for removing a minimizing technology for the vitriol that material produces in supercritical water oxidation process, it is characterized in that, described minimizing technology comprises:
Material is added and agglomerator carries out supercritical water oxidation process in supercritical reaction device; Described agglomerator is the agglomerator described in any one of claim 1 to 5;
Remove the composite aggregate being deposited in described supercritical reaction device bottom.
7. minimizing technology according to claim 6, is characterized in that, the add-on of described agglomerator is 2.8 ~ 3.1 times of the element sulphur quality that described material comprises.
8. minimizing technology according to claim 6, is characterized in that, the particle diameter span of the described composite aggregate of formation is 1 ~ 6mm.
9. minimizing technology according to claim 6, is characterized in that, described removal is deposited in the composite aggregate of described supercritical reaction device bottom, specifically comprises:
Reduce the temperature of described supercritical reaction device bottom, make the vitriol in described composite aggregate be dissolved in the aqueous solution, the insoluble substance including the insoluble compound in described composite aggregate is gathered in the bottom of described supercritical reaction device bottom;
The bottom giving off described supercritical reaction device bottom is dissolved with the aqueous solution of described vitriol and the described insoluble substance of gathering.
10. minimizing technology according to claim 9, is characterized in that, the temperature of described supercritical reaction device bottom is reduced to and is more than or equal to room temperature and is less than 100 DEG C.
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| US20140246371A1 (en) * | 2013-03-01 | 2014-09-04 | Baker Hughes Incorporated | Process for removing sulfate and system for same |
| CN104370392A (en) * | 2014-12-03 | 2015-02-25 | 广州蓝涛水处理有限公司 | Treatment method for smelting waste water containing sulfuric acid and heavy metal |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140246371A1 (en) * | 2013-03-01 | 2014-09-04 | Baker Hughes Incorporated | Process for removing sulfate and system for same |
| CN104370392A (en) * | 2014-12-03 | 2015-02-25 | 广州蓝涛水处理有限公司 | Treatment method for smelting waste water containing sulfuric acid and heavy metal |
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Effective date of registration: 20180102 Address after: 065001 Hebei city of Langfang province C New Austrian Science Park Economic Development Zone Xinyuan host city Patentee after: Environmental Protection Technology Co., Ltd. Address before: The 065001 Hebei economic and Technological Development Zone of Langfang Huaxiang new Austrian Science and Technology Park in the Southern District B building room 522 Patentee before: ENN SCIENCE & TECHNOLOGY DEVELOPMENT Co.,Ltd. |