CN109455737B - Method for recovering sodium chloride and calcium chloride from waste dechlorinating agent - Google Patents

Method for recovering sodium chloride and calcium chloride from waste dechlorinating agent Download PDF

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Publication number
CN109455737B
CN109455737B CN201710796394.XA CN201710796394A CN109455737B CN 109455737 B CN109455737 B CN 109455737B CN 201710796394 A CN201710796394 A CN 201710796394A CN 109455737 B CN109455737 B CN 109455737B
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waste
dechlorinating agent
filter cake
mass
filtrate
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CN109455737A (en
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王继元
卞伯同
邵林红
堵文斌
孟海
王亚明
杨爱武
朱庆奋
柏基业
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China Petroleum and Chemical Corp
Sinopec Yangzi Petrochemical Co Ltd
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Sinopec Yangzi Petrochemical Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D3/00—Halides of sodium, potassium or alkali metals in general
    • C01D3/04—Chlorides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00—Compounds of calcium, strontium, or barium
    • C01F11/20—Halides
    • C01F11/24—Chlorides
    • C01F11/28—Chlorides by chlorination of alkaline-earth metal compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

The invention disclosesA method for recovering sodium chloride and calcium chloride from a waste dechlorinating agent adopts a step-by-step neutralization method, firstly controls the pH value to be 7-8, and enables concentrated hydrochloric acid and Na in the waste dechlorinating agent2O preferentially reacts to generate NaCl, and the NaCl is recovered through operations such as filtration, evaporation and the like; and controlling the pH value to be 6-7, so that concentrated hydrochloric acid reacts with CaO in the waste dechlorinating agent to generate CaCl2Recovering CaCl by filtration, evaporation, etc2. The invention has simple operation process, and the recovered NaCl and CaCl2The purity of the dechlorinating agent is very high, and the resource utilization of the waste dechlorinating agent is realized; the quantity of the solid slag obtained by recycling is less, and the reduction of the waste dechlorinating agent is realized.

Description

Method for recovering sodium chloride and calcium chloride from waste dechlorinating agent
Technical Field
The invention relates to a method for recycling a waste dechlorinating agent.
Background
More force is input in the research aspect of dechlorinating agents at home and abroad, and various patent technologies and reports emerge endlessly. From the literature reports, HCl is mainly removed from naphtha, light liquid hydrocarbon and liquefied petroleum gas at present.
The waste dechlorinating agent belongs to dangerous solid waste, and the treatment standard and the treatment difficulty of industrial solid waste are high. At present, the conventional treatment methods of industrial solid wastes generally comprise a landfill method, a burning method and the like, when the industrial solid wastes are treated by the landfill method, a dangerous waste landfill site with higher standard needs to be built, but with the speed of urbanization, the site selection of the landfill site becomes more difficult. When industrial solid waste is treated by the incineration method, because the components are complex, a lot of toxic and harmful substances are easily generated, a special industrial garbage incinerator is often used for treatment, the treatment components are high, and secondary pollution can be generated.
At present, the treatment of the waste dechlorinating agent usually adopts a landfill method, the treatment cost is higher, and the underground water body is easily polluted due to improper treatment. The resource utilization of the waste dechlorinating agent is still in a blank stage.
Typical spent dechlorinating agents are shown in Table 1 in terms of composition and content. As can be seen, the effective active ingredients of the dechlorinating agent are CaO and Na2O, Cl content in the waste dechlorinating agent is as high as 13.1%, only the composition with content more than 0.1% is listed in the table, and the others are not listed.
TABLE 1 typical composition and content of spent dechlorinating agent
Figure GDA0002847619400000011
Disclosure of Invention
In order to overcome the defects that the waste dechlorinating agent cannot be utilized and the like in the prior art, the invention provides a method for recovering sodium chloride and calcium chloride from the waste dechlorinating agent.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a method for recovering sodium chloride and calcium chloride from waste dechlorinating agent comprises the following steps in sequence:
(1) crushing the waste dechlorinating agent into 100-300 meshes, adding the crushed waste dechlorinating agent into water at the temperature of 0-100 ℃, and stirring the mixture for 0.1-10 hours at the stirring speed of 500 +/-100 r/min to obtain a slurry material I, wherein the mass of the water is 0.5-5 times that of the waste dechlorinating agent;
(2) adding concentrated hydrochloric acid into the slurry material I obtained in the step (1) in the continuous stirring process, neutralizing until the pH value is 7-8, filtering and washing to obtain a filtrate I and a filter cake I, and evaporating the filtrate I to obtain NaCl;
(3) adding water with the temperature of 0-100 ℃ into the filter cake I obtained in the step (2), and stirring for 0.1-10 hours to obtain a slurry material II, wherein the mass of the water is 0.5-5 times that of the filter cake I;
(4) adding concentrated hydrochloric acid into the slurry material II obtained in the step (3) in the continuous stirring process, neutralizing until the pH value is 6-7, and filtering and washing to obtain a filtrate II and a filter cake II; evaporating the filtrate II to obtain CaCl2(ii) a And drying the filter cake II to obtain solid slag.
The application follows from Na2The difficulty degree of the neutralization reaction of O, CaO and hydrochloric acid is controlled to be 7-8 by adopting a step-by-step neutralization method, so that concentrated hydrochloric acid and Na in the waste dechlorinating agent2O preferentially reacts to generate NaCl, and the NaCl is recovered through operations such as filtration, evaporation and the like; and controlling the pH value to be 6-7, so that concentrated hydrochloric acid reacts with CaO in the waste dechlorinating agent to generate CaCl2Recovering CaCl by filtration, evaporation, etc2。
In order to improve the recycling rate and recovery purity of NaCl, in the step (1), the temperature of water is 10-70 ℃; the mass of the water is 1-3 times of that of the waste dechlorinating agent; the stirring time is 1-5 h.
In the step (2) and the step (4), the mass concentration of the concentrated hydrochloric acid is 36.5%, and the evaporation temperature of the filtrate in the step (2) is 100-150 ℃.
In the step (2), the mass purity of the obtained NaCl is 90-95%.
To improve CaCl2The recycling rate and the recovery purity of the filter cake I are improved, in the step (3), the temperature of water is 10-70 ℃, the mass of the water is 1-3 times of that of the filter cake I, and the stirring time is 1-5 hours.
In order to improve the product purity and the production efficiency, in the step (4), the evaporation temperature is 100-150 ℃.
In the above step (4), CaCl2The mass purity of (A) is 95-99%.
In the step (4), the mass of the solid slag is 20-40% of that of the waste dechlorinating agent.
The prior art is referred to in the art for techniques not mentioned in the present invention.
The invention is from wasteThe method for recovering sodium chloride and calcium chloride from dechlorinating agent has simple operation process, and the recovered NaCl and CaCl2The purity of the dechlorinating agent is very high, and the resource utilization of the waste dechlorinating agent is realized; the quantity of the solid slag obtained by recycling is less, and the reduction of the waste dechlorinating agent is realized.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
Example 1
(1) Crushing 100g of spherical waste dechlorinating agent to 100 meshes, adding the spherical waste dechlorinating agent into 0 ℃ tap water, and continuously stirring the mixture for 10 hours at the stirring speed of 500r/min to obtain a pasty material I, wherein the mass of the tap water is 0.5 time of that of the waste dechlorinating agent;
(2) adding concentrated hydrochloric acid (the mass concentration of the concentrated hydrochloric acid is 36.5%) into the slurry material I obtained in the step (1) in the continuous stirring process, neutralizing until the pH value is 7, and filtering and washing to obtain a filtrate I and a filter cake I; evaporating the filtrate I to obtain NaCl;
(3) adding tap water with the temperature of 0 ℃ into the filter cake I obtained in the step (2), and continuously stirring for 10 hours to obtain a slurry-like material II, wherein the mass of the tap water is 0.5 time that of the filter cake I;
(4) adding concentrated hydrochloric acid (the mass concentration is 36.5%) into the slurry material II obtained in the step (3) in the process of continuously stirring (500r/min), neutralizing until the pH value is 6, and filtering and washing to obtain a filtrate II and a filter cake II; evaporating the filtrate II to obtain CaCl2(ii) a And drying the filter cake II to obtain solid slag.
NaCl and CaCl obtained in this example2The purity and the mass ratio of the solid slag to the waste dechlorinating agent are shown in the table 2.
Example 2
(1) Crushing 100g of spherical waste dechlorinating agent to 300 meshes, adding the spherical waste dechlorinating agent into tap water at the temperature of 100 ℃, and continuously stirring the mixture for 0.1 hour under the condition of the stirring speed of 500r/min to obtain a pasty material I, wherein the mass of the tap water is 5 times that of the waste dechlorinating agent;
(2) adding concentrated hydrochloric acid (the mass concentration is 36.5%) into the slurry material I obtained in the step (1) in the continuous stirring process, neutralizing until the pH value is 8, and filtering and washing to obtain a filtrate I and a filter cake I; evaporating the filtrate I to obtain NaCl;
(3) adding tap water with the temperature of 100 ℃ into the filter cake I obtained in the step (2), and continuously stirring for 0.1h to obtain a slurry-like material II, wherein the mass of the tap water is 5 times that of the filter cake I;
(4) adding concentrated hydrochloric acid (the mass concentration is 36.5%) into the slurry material II obtained in the step (3) in the stirring process of continuously stirring (500r/min), neutralizing until the pH value is 7, and filtering and washing to obtain a filtrate II and a filter cake II; evaporating the filtrate II to obtain CaCl2(ii) a And drying the filter cake II to obtain solid slag.
NaCl and CaCl obtained in this example2The purity and the mass ratio of the solid slag to the waste dechlorinating agent are shown in the table 2.
Example 3
(1) Crushing 100g of spherical waste dechlorinating agent to 200 meshes, adding the spherical waste dechlorinating agent into 10 ℃ tap water, and continuously stirring the mixture for 1 hour under the condition of a stirring speed of 500r/min to obtain a pasty material I, wherein the mass of the tap water is 1 time of that of the waste dechlorinating agent;
(2) adding concentrated hydrochloric acid (the mass concentration is 36.5%) into the slurry material I obtained in the step (1) in the continuous stirring process, neutralizing until the pH value is 7, and filtering and washing to obtain a filtrate I and a filter cake I; evaporating the filtrate I to obtain NaCl;
(3) adding tap water with the temperature of 10 ℃ into the filter cake I obtained in the step (2), and continuously stirring for 1h to obtain a slurry-like material II, wherein the mass of the tap water is 1 time that of the filter cake I;
(4) adding concentrated hydrochloric acid (the mass concentration is 36.5%) into the slurry material II obtained in the step (3) in the process of continuously stirring (500r/min), neutralizing until the pH value is 6, and filtering and washing to obtain a filtrate II and a filter cake II; evaporating the filtrate II to obtain CaCl2(ii) a And drying the filter cake II to obtain solid slag.
NaCl and CaCl obtained in this example2The purity and the mass ratio of the solid slag to the waste dechlorinating agent are shown in the table 2.
Example 4
(1) Crushing 100g of spherical waste dechlorinating agent to 200 meshes, adding the spherical waste dechlorinating agent into tap water at 70 ℃, and continuously stirring the mixture for 5 hours at the stirring speed of 500r/min to obtain a pasty material I, wherein the mass of the tap water is 3 times that of the waste dechlorinating agent;
(2) adding concentrated hydrochloric acid (the mass concentration is 36.5%) into the slurry material I obtained in the step (1) in the continuous stirring process, neutralizing until the pH value is 7, and filtering and washing to obtain a filtrate I and a filter cake I; evaporating the filtrate I to obtain NaCl;
(3) adding tap water with the temperature of 70 ℃ into the filter cake I obtained in the step (2), and continuously stirring for 5 hours to obtain a slurry-like material II, wherein the mass of the tap water is 3 times that of the filter cake I;
(4) adding concentrated hydrochloric acid (the mass concentration is 36.5%) into the slurry material II obtained in the step (3) in the process of continuously stirring (500r/min), neutralizing until the pH value is 6, and filtering and washing to obtain a filtrate II and a filter cake II; evaporating the filtrate II to obtain CaCl2(ii) a And drying the filter cake II to obtain solid slag.
NaCl and CaCl obtained in this example2The purity and the mass ratio of the solid slag to the waste dechlorinating agent are shown in the table 2.
Example 5
(1) Crushing 100g of spherical waste dechlorinating agent to 200 meshes, adding the spherical waste dechlorinating agent into tap water at the temperature of 30 ℃, and continuously stirring the mixture for 2 hours at the stirring speed of 500r/min to obtain a pasty material I, wherein the mass of the tap water is 1 time of that of the waste dechlorinating agent;
(2) adding concentrated hydrochloric acid (the mass concentration is 36.5%) into the slurry material I obtained in the step (1) in the continuous stirring process, neutralizing until the pH value is 7.5, and filtering and washing to obtain a filtrate I and a filter cake I; evaporating the filtrate I to obtain NaCl;
(3) adding tap water with the temperature of 30 ℃ into the filter cake I obtained in the step (2), and continuously stirring for 2 hours to obtain a slurry-like material II, wherein the mass of the tap water is 2 times that of the filter cake I;
(4) adding concentrated hydrochloric acid (mass concentration is 36.5%) into the slurry material II obtained in the step (3) while continuously stirring (500r/min), neutralizing until the pH value is 6.5, and performingFiltering and washing to obtain filtrate II and filter cake II; evaporating the filtrate II to obtain CaCl2(ii) a And drying the filter cake II to obtain solid slag.
NaCl and CaCl obtained in this example2The purity and the mass ratio of the solid slag to the waste dechlorinating agent are shown in the table 2.
Example 6
(1) Crushing 100g of spherical waste dechlorinating agent into 200 meshes, adding the spherical waste dechlorinating agent into tap water at the temperature of 50 ℃, and continuously stirring the mixture for 1.5 hours under the condition of the stirring speed of 500r/min to obtain a pasty material I, wherein the mass of the tap water is 2 times that of the waste dechlorinating agent;
(2) adding concentrated hydrochloric acid (the mass concentration is 36.5%) into the slurry material I obtained in the step (1) in the continuous stirring process, neutralizing until the pH value is 7.5, and filtering and washing to obtain a filtrate I and a filter cake I; evaporating the filtrate I to obtain NaCl;
(3) adding tap water with the temperature of 50 ℃ into the filter cake I obtained in the step (2), and continuously stirring for 2 hours to obtain a slurry-like material II, wherein the mass of the tap water is 2 times that of the filter cake I;
(4) adding concentrated hydrochloric acid (the mass concentration is 36.5%) into the slurry material II obtained in the step (3) in the process of continuously stirring (500r/min), neutralizing until the pH value is 6.5, and filtering and washing to obtain a filtrate II and a filter cake II; evaporating the filtrate II to obtain CaCl2(ii) a And drying the filter cake II to obtain solid slag.
NaCl and CaCl obtained in this example2The purity and the mass ratio of the solid slag to the waste dechlorinating agent are shown in the table 2.
Example 7
(1) Crushing 100g of spherical waste dechlorinating agent to 200 meshes, adding the spherical waste dechlorinating agent into tap water at the temperature of 30 ℃, and continuously stirring the mixture for 2 hours at the stirring speed of 500r/min to obtain a pasty material I, wherein the mass of the tap water is 1 time of that of the waste dechlorinating agent;
(2) adding concentrated hydrochloric acid (the mass concentration is 36.5%) into the slurry material I obtained in the step (1) in the continuous stirring process, neutralizing until the pH value is 8, and filtering and washing to obtain a filtrate I and a filter cake I; evaporating the filtrate I to obtain NaCl;
(3) adding tap water with the temperature of 50 ℃ into the filter cake I obtained in the step (2), and continuously stirring for 2 hours to obtain a slurry-like material II, wherein the mass of the tap water is 1 time that of the filter cake I;
(4) adding concentrated hydrochloric acid (the mass concentration is 36.5%) into the slurry material II obtained in the step (3) in the process of continuously stirring (500r/min), neutralizing until the pH value is 6, and filtering and washing to obtain a filtrate II and a filter cake II; evaporating the filtrate II to obtain CaCl2(ii) a And drying the filter cake II to obtain solid slag.
NaCl and CaCl obtained in this example2The purity and the mass ratio of the solid slag to the waste dechlorinating agent are shown in the table 2.
Example 8
(1) Crushing 100g of spherical waste dechlorinating agent to 200 meshes, adding the spherical waste dechlorinating agent into tap water at 60 ℃, and continuously stirring the mixture for 2 hours at the stirring speed of 500r/min to obtain a pasty material I, wherein the mass of the tap water is 1 time of that of the waste dechlorinating agent;
(2) adding concentrated hydrochloric acid (the mass concentration is 36.5%) into the slurry material I obtained in the step (1) in the continuous stirring process, neutralizing until the pH value is 8, and filtering and washing to obtain a filtrate I and a filter cake I; evaporating the filtrate I to obtain NaCl;
(3) adding tap water with the temperature of 30 ℃ into the filter cake I obtained in the step (2), and continuously stirring for 1h to obtain a slurry-like material II, wherein the mass of the tap water is 2 times that of the filter cake I;
(4) adding concentrated hydrochloric acid (the mass concentration is 36.5%) into the slurry material II obtained in the step (3) in the process of continuously stirring (500r/min), neutralizing until the pH value is 6, and filtering and washing to obtain a filtrate II and a filter cake II; evaporating the filtrate II to obtain CaCl2(ii) a And drying the filter cake II to obtain solid slag.
NaCl and CaCl obtained in this example2The purity and the mass ratio of the solid slag to the waste dechlorinating agent are shown in the table 2.
Comparative example 1
Compared with the embodiment 5, NaCl and CaCl are recovered by adopting a one-step neutralization method2。
(1) Crushing 100g of spherical waste dechlorinating agent to 200 meshes, adding the spherical waste dechlorinating agent into tap water at the temperature of 30 ℃, and continuously stirring the mixture for 2 hours at the stirring speed of 500r/min to obtain a pasty material I, wherein the mass of the tap water is 1 time of that of the waste dechlorinating agent;
(2) adding concentrated hydrochloric acid (the mass concentration is 36.5%) into the slurry material I obtained in the step (1) in the process of continuously stirring (500r/min), neutralizing until the pH value is 6.5, and filtering and washing to obtain a filtrate I and a filter cake I; evaporating the filtrate I to obtain NaCl and CaCl2(ii) a And drying the filter cake I to obtain solid slag.
NaCl and CaCl obtained in this comparative example2The purity and the mass ratio of the solid slag to the waste dechlorinating agent are shown in the table 2.
In comparison of the embodiment and the comparative example, the invention adopts a step-by-step neutralization method, firstly recovers NaCl, and the purity of the NaCl is as high as 90-95%; then recycling CaCl2The purity of the product is as high as 95-99%. And NaCl and CaCl are recovered by adopting a one-step neutralization method2NaCl purity of only 73%, CaCl2The purity of (A) is only 80%, which represents the superiority of the method of the invention.
TABLE 2 NaCl, CaCl2The purity of the dechlorinating agent is higher than that of the solid slag
Figure GDA0002847619400000061
Figure GDA0002847619400000071

Claims (10)

1. A method for recovering sodium chloride and calcium chloride from waste dechlorinating agent is characterized by comprising the following steps: comprises the following steps that:
(1) crushing the waste dechlorinating agent into 100-300 meshes, adding the crushed waste dechlorinating agent into water at the temperature of 0-100 ℃, and stirring the mixture for 0.1-10 hours at the stirring speed of 500 +/-100 r/min to obtain a slurry material I, wherein the mass of the water is 0.5-5 times that of the waste dechlorinating agent;
(2) adding concentrated hydrochloric acid into the slurry material I obtained in the step (1) in the continuous stirring process, neutralizing until the pH value is 7-8, filtering and washing to obtain a filtrate I and a filter cake I, and evaporating the filtrate I to obtain NaCl;
(3) adding water with the temperature of 0-100 ℃ into the filter cake I obtained in the step (2), and stirring for 0.1-10 hours to obtain a slurry material II, wherein the mass of the water is 0.5-5 times that of the filter cake I;
(4) adding concentrated hydrochloric acid into the slurry material II obtained in the step (3) in the continuous stirring process, neutralizing until the pH value is 6-7, and filtering and washing to obtain a filtrate II and a filter cake II; evaporating the filtrate II to obtain CaCl2(ii) a And drying the filter cake II to obtain solid slag.
2. The method of claim 1, wherein: in the step (1), the temperature of the water is 10-70 ℃.
3. The method of claim 1 or 2, wherein: in the step (1), the mass of water is 1-3 times of that of the waste dechlorinating agent.
4. The method of claim 1 or 2, wherein: in the step (1), the stirring time is 1-5 h.
5. The method of claim 1 or 2, wherein: in the step (2), the mass purity of the obtained NaCl is 90-95%.
6. The method of claim 1 or 2, wherein: in the step (3), the temperature of the water is 10-70 ℃.
7. The method of claim 1 or 2, wherein: in the step (3), the mass of water is 1-3 times of that of the filter cake I.
8. The method of claim 1 or 2, wherein: in the step (3), the stirring time is 1-5 h.
9. A method as claimed in claim 1 or 2The method is characterized in that: in step (4), CaCl2The mass purity of (A) is 95-99%.
10. The method of claim 1 or 2, wherein: in the step (4), the mass of the solid slag is 20-40% of that of the waste dechlorinating agent.
CN201710796394.XA 2017-09-06 2017-09-06 Method for recovering sodium chloride and calcium chloride from waste dechlorinating agent Active CN109455737B (en)

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