CN114477236B - Calcium halide purifying method and pH value adjusting method - Google Patents
Calcium halide purifying method and pH value adjusting method Download PDFInfo
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- CN114477236B CN114477236B CN202210104146.5A CN202210104146A CN114477236B CN 114477236 B CN114477236 B CN 114477236B CN 202210104146 A CN202210104146 A CN 202210104146A CN 114477236 B CN114477236 B CN 114477236B
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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
- C01D3/06—Preparation by working up brines; seawater or spent lyes
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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
- C01D3/14—Purification
- C01D3/16—Purification by precipitation or adsorption
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- 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
- C01F11/32—Purification
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Abstract
The application relates to a method for purifying calcium brine and a method for adjusting pH value, wherein the method for purifying S1 comprises the steps of taking single-well calcium brine, detecting the calcium brine, and detecting NaCl and CaCl 2 The method comprises the steps of carrying out a first treatment on the surface of the Introducing the calcium brine into a raw brine barrel, and detecting the calcium brine in the raw brine barrel, wherein the detection items comprise: naCl, caCl 2 、Mg 2+ Content and pH value. S2, determining the weight of lime powder according to the data detected in the raw brine barrel in the step S1; lime powder and refined brine are mixed to obtain lime milk, and the problem that the lime milk calcium brine is purified and the pH value is controlled before the brine enters an evaporation system is solved by the application.
Description
Technical Field
The application relates to the field of inorganic chemical industry, in particular to a calcium halide purifying method and a pH value adjusting method.
Background
In the production of salt calcium, the pH value of the calcium halide should be 10.5-11, and the existing calcium halide contains no or trace magnesium ions, but the existing calcium halide is generally alkalescent, the pH value is far lower than the above value, and the magnesium ion content is higher. In order to reduce the adverse effects of low pH value of the calcium halide on corrosion of equipment pipelines in salt calcium production and the like, the pH value is often required to be adjusted to be 10.5-11 so as to improve the alkalinity of the calcium halide, and in order to prevent magnesium ions from being separated out into scale layers to be attached to the equipment pipelines in salt calcium production, heat transfer is affected or the pipe diameter is reduced, the calcium halide brine is often required to be purified so as to remove magnesium.
Common raw materials for purifying and removing magnesium and improving the pH value of the calcium halide are as follows: liquid caustic soda or quicklime. The liquid caustic soda and the calcium halide are directly used for purifying and regulating the pH value, a liquid caustic soda storage tank, a caustic soda pump, a matched pipeline, an electric instrument, civil engineering and other equipment are needed, the rest of the liquid caustic soda with the content of 32% is water, namely, a large amount of clear water enters a salt-calcium device evaporation system by taking the liquid caustic soda as a raw material, the raw material of the calcium halide is not purified and pretreated, scaling is easy to occur, heat transfer is influenced, the price of the liquid caustic soda is higher than that of the quicklime, and the production cost is very high; the pH value can be adjusted by the quicklime to be used in the calcium brine before the evaporation system, the stability of the active ingredients of the quicklime is poor, the addition amount is difficult to control, more water-insoluble impurities enter the evaporation system to influence the product quality, the raw pretreatment of the calcium brine is easy to scale and influence the heat transfer, the facility investment is more, a lime storage barrel, a lime dissolving barrel and a lime milk pump are needed to be newly added or utilized, and the cost of matched pipelines, electric instruments and civil engineering is high.
Disclosure of Invention
Based on the problems, the application aims to provide a method for purifying calcium halide and a method for adjusting pH value in the production of salt calcium, which solves the problems caused by the fact that raw water enters an evaporation system more than in the prior art, water insoluble impurities enter a production device more than in the prior art, the quality of the product is affected, the operation difficulty is high, and the like;
in order to achieve the above object, the present application provides the following technical solutions:
in one aspect, the application provides a method for purifying calcium halide in salt calcium production,
the method comprises the following steps:
s1, taking single-well calcium brine, and detecting the calcium brine, including detecting NaCl and CaCl 2 The method comprises the steps of carrying out a first treatment on the surface of the Introducing the calcium brine into a raw brine barrel, and detecting the calcium brine in the raw brine barrel, wherein the detection items comprise: naCl, caCl 2 、Mg 2+ Content and pH value;
s2, according to the data detected in the raw brine barrel in the step S1,
determining the weight of lime powder; mixing lime powder with refined brine to obtain lime milk;
s3, mixing the calcium brine in the raw brine barrel in the step S1 with the lime milk obtained in the step S2 in a reaction barrel, and adding a flocculating agent after the reaction is completed.
Preferably, the step S1 includes the steps of:
s11, taking a single-well calcium halide sample, and analyzing and detecting NaCl and CaCl of each single-well calcium halide 2 ；
S12, feeding the calcium brine single-well brine into a calcium brine raw brine barrel, and calculating the total raw brine hour flow, wherein if the raw brine flow is more than 560m 3 /h; when the liquid level reaches 3 meters, starting the stirring device;
s13, if the flow of the raw halogen is lower than 560m 3 /h, caCl by calcium halide 2 And sodium nitrohalogenide Na 2 SO 4 Adding the difference of the supplementing calcium halogen amount;
s14, when the liquid level of the raw brine barrel reaches 14 meters, starting a raw brine pump to transfer materials to the reaction barrel, stopping transferring materials when the liquid level reaches 19.5 meters, and recording the liquid level of the reaction barrel; starting a stirring device matched with the reaction barrel when the feed liquid is 3 meters;
s15, taking a raw brine barrel calcium brine sample for analysis and detection of NaCl and CaCl of the calcium brine 2 pH value, mg 2+ The content is as follows.
Preferably, the configuration of the lime milk comprises the following steps:
s1, automatically flowing lime powder to a lime metering scale, and weighing the weight of the lime powder required by calcium halide purification.
S2, enabling refined brine to flow into a lime milk preparing barrel, adding lime powder into the lime milk preparing barrel, stirring, and continuously stirring to enable the lime powder to be dissolved and emulsified into lime milk for later use.
Preferably, the step S3 specifically includes the following steps:
s31, adding lime milk into the reaction barrel, and mixing and stirring with calcium halide in the reaction barrel;
s32, performing brine purification reaction;
s33, detecting the pH value of the calcium halide after stirring and reacting for 3 hours in a reaction barrel.
And S34, if the pH value of the detected calcium halide is not lower than 10.5, adding the prepared flocculating agent into a reaction barrel, stopping the flocculating agent preparing barrel stirring device, and stopping stirring after the stirring device in the reaction barrel continuously stirs for 5 minutes.
S35, after the reaction barrel is clarified for 3 hours by stopping the stirring device, detecting calcium halide in the reaction barrel, wherein the detection items comprise: naCl, caCl 2 pH value and solid matter.
Preferably, the adjusting method further includes, after step S3:
s4, after the clear and halogen-removing of the reaction barrel is detected to be qualified, the clear halogen in the reaction barrel is transferred to a refined halogen barrel;
s5, conveying clear brine in the fine brine barrel in the step S4 to a calcium brine barrel of a brine purifying workshop to serve as a raw material of a salt calcium production device.
Preferably, after the halogen cleaning and transferring in the reaction barrel to the refined halogen barrel, the method further comprises the following steps:
s41, after the halogen clearing and material transferring of the reaction barrel are completed, stirring is started, and the reaction magnesium mud is stirred into a suspension state;
s42, after the reaction magnesium mud is uniformly stirred, conveying the mud to a light calcium liquid barrel, and injecting the light calcium liquid into a well to produce brine.
In yet another aspect, the present application provides a method of pH adjustment, the method comprising the steps of:
s21, according to the liquid level of the calcium halide in the reaction barrel, mg 2+ Calculating the weight of lime powder required by removing magnesium from calcium halide by the content and the CaO and MgO contents of the lime powder;
s22, calculating the weight of lime powder required by adjusting the pH value of the calcium halide according to the liquid level and the pH value of the calcium halide in the reaction barrel and the pH value adjusted to be not lower than 10.5; the sum of the weights of lime powder required by the calcium halide magnesium removal and the pH value adjustment is the weight of lime powder required by the calcium halide purification of the batch.
S23, calculating the weight of lime powder
The formula of the lime powder by weight is as follows:
m (CaO) ＝(230.73×c (Mg2+) +8.8666)×h÷ω (CaO)
wherein: m is m (CaO) Lime powder weight, unit/(Kg) is added for calcium halide purification and pH adjustment
c (Mg2+) -magnesium content in the calcium halide in units/(g/L)
V- - -volume of reaction barrel (T-1181B/C) calcium halide, unit/(m) 3 )
ω (CaO) Measuring the effective calcium oxide content of the lime powder, unit/(%)
In yet another aspect, the present application provides an apparatus for a method of adjusting the pH of a calcium halide in the production of calcium salts comprising: a calcium bittern raw brine barrel, a reaction barrel, a fine bittern barrel, a flocculating agent preparation barrel, a lime milk preparation barrel and a light calcium solution barrel;
the calcium brine raw brine barrel is used for collecting and storing calcium brine raw brine, the calcium brine raw brine enters the calcium brine raw brine barrel from the brine well through a pipeline, and the total flow of raw brine hours is calculated (T-1181A);
the reaction barrel is used for purifying and reacting the calcium halide raw halogen and adjusting the pH value, the reaction barrel is connected with the calcium halide raw halogen barrel through a pipeline, and a raw halogen pump is arranged on the pipeline between the reaction barrel and the calcium halide raw halogen barrel;
the refined brine barrel is used for storing refined brine, the refined brine barrel is connected with the reaction barrel through a pipeline, and a brine cleaning pump is arranged on the pipeline between the refined brine barrel and the reaction barrel;
the flocculant preparation barrel is used for preparing and storing flocculant, a flocculant pump is arranged on a pipeline between the flocculant preparation barrel and the reaction barrel which are connected through a pipeline, and a denitration calcium halide pump is arranged on a pipeline between the flocculant preparation barrel and the refined halogen barrel which are connected through a pipeline;
the lime milk preparing barrel is used for preparing and storing lime milk, and a denitration calcium brine pump is arranged on a pipeline between the lime milk preparing barrel and the fine brine barrel through a pipeline; a lime milk pump is arranged on the pipeline between the lime milk preparing barrel and the reaction barrel through the pipeline;
the light calcium solution barrel is used for storing light calcium solution, and a slurry pump is arranged on a pipeline between the light calcium solution barrel and the reaction barrel which are connected through a pipeline.
Compared with the prior art, the application has the following beneficial effects:
the pipeline of the equipment is changed less, so that the utilization rate of part of the existing equipment can be improved; the device is placed together with nitrate brine purification and the like, has strong integrity, is convenient for centralized management, and is beneficial to operation;
the application solves the problems of purifying calcium brine by lime milk and adjusting pH on the well, and stabilizing and adjusting pH.
Drawings
Fig. 1: is a schematic diagram of the equipment of the method for purifying the calcium halide in the production of the salt calcium in the specific embodiment of the application.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present application more apparent, the technical solutions of the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments of the present application. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
The application relates to a method for purifying calcium halide in salt calcium production and a method for adjusting pH value, wherein the connection relation of equipment is shown in figure 1
The equipment comprises a calcium brine raw brine barrel, a reaction barrel, a refined brine barrel, a flocculating agent preparation barrel, a lime milk preparation barrel and a light calcium solution barrel as seen in fig. 1;
the calcium brine raw brine barrel obtains raw brine from a brine well, and the raw brine enters a reaction barrel through a pipeline; the reaction barrel is communicated with the flocculant preparation barrel and the lime milk preparation barrel, calcium halide is purified by the reaction of lime milk and the raw halide, the pH value is regulated to a standard value, and then the flocculant is added for separating impurities; the reaction barrel is also communicated with a refined brine barrel, brine with the pH value reaching a standard value and removed of impurities is introduced into the refined brine barrel from the reaction barrel, the refined brine barrel is also connected with a lime milk preparation barrel and a flocculant preparation barrel, and refined brine is introduced into the lime milk preparation barrel and the flocculant preparation barrel for preparing lime milk and flocculant; and then the reaction barrel is connected with the light calcium liquid barrel, the precipitated impurities are introduced into the light calcium liquid barrel, the main components of the impurities are magnesium hydroxide precipitate and water insoluble matters in quick lime, and the impurities can be directly used for exploiting raw halogen after being mixed with the light calcium liquid.
Each barrel is connected through a pipeline, and is provided with a corresponding valve and a pump, and an adaptive stirring device is arranged in each barrel.
The method for increasing the pH value of the calcium halide is compared with the following table 1
TABLE 1
Example 1
In example 1, the room temperature of the reaction environment is 25 ℃, and all barrel specifications of a raw brine barrel, a reaction barrel, a refined brine barrel and the like are phi 20000 multiplied by 22000.
1.1 raw brine preparation
1) Taking a single-well calcium bittern sample, analyzing and monitoring NaCl of each single-well calcium bittern、CaCl 2 。
2) Blending the raw brine mass and the brine number of the calcium brine wells, feeding the calcium brine single well brine into a calcium brine raw brine barrel (T-1181A), calculating the total flow of raw brine hours, and keeping the raw brine yield to be more than 560m 3 /h; when the liquid level reached 3 meters, the stirring device (AG-1181A) was turned on.
3) If the flow rate of the raw halogen is lower than 560m 3 According to calcium halide CaCl 2 And sodium nitrohalogenide Na 2 SO 4 The difference of the calcium halogen amount is compensated.
4) When the liquid level of the raw brine barrel A (T-1181A) reaches 14 meters, starting a raw brine pump (P-1181) according to a regulation, transferring materials to a reaction barrel (T-1181B/C) until the liquid level reaches 19.5 meters, stopping transferring materials, stopping pumping according to the regulation, and recording the liquid level of the reaction barrel; when the feed liquid is 3 meters, a stirring device (AG-1181B/C) matched with the reaction barrel is started.
5) The laboratory staff takes a raw bittern barrel (T-1181A) according to the regulations to analyze and monitor NaCl and CaCl of the calcium bittern 2 pH value, mg 2 + The content is as follows.
1.2 lime milk preparation
1.2.1 lime powder weight calculation
1) According to the liquid level and Mg of the calcium halide in the reaction barrel 2+ The content, and the CaO and MgO contents of the lime powder calculate the weight of the lime powder required by removing magnesium from the calcium halide.
2) And calculating the weight of lime powder required by regulating the pH value of the calcium halide according to the liquid level and the pH value of the calcium halide in the reaction barrel and the standard reaching value of the refined halogen pH value of 10.5.
3) The sum of the weights of lime powder required by the calcium halide magnesium removal and the pH value adjustment is the weight of lime powder required by the calcium halide purification of the batch.
4) Lime powder weight calculation
The weight formula of lime powder to be added for purifying and adjusting pH of calcium halide in each reaction barrel is as follows:
m (CaO) ＝(72447×c (Mg2+) +2784.11)×h÷ω (CaO)
wherein: m is m (CaO) Lime powder weight, unit/(Kg) is added for calcium halide purification and pH adjustment
c (Mg2+) -magnesium content in the calcium halide in units/(g/L)
h- - -reaction barrel (T-1181B/C) calcium halide level, unit/(m)
ω (CaO) Measuring the effective calcium oxide content of the lime powder, unit/(%)
1.2.2 preparation of lime milk
1) The lime powder automatically flows from the lime bin to a lime metering scale, and the weight of lime powder required by the batch of calcium halide purification is weighed.
2) Opening a valve from the refined brine barrel (T-1181D) to a lime milk preparation barrel pipeline, and enabling refined brine to flow to the lime milk preparation barrel (T-1184) or adding refined brine into the lime milk preparation barrel by a denitration calcium brine pump (P-1184A/B) when the liquid level of the refined brine barrel is low, and stopping adding refined brine when the liquid level reaches 3.5 meters; when the feed liquid reaches 1 meter, a stirring device (AG-1184) of the lime milk preparing barrel is started.
3) When the refined brine is added into the lime milk preparing barrel (T-1184) to the liquid level of 1.5 m, the screw conveyor is started to add the lime powder weighed in the metering scale into the lime milk preparing barrel (T-1184), and the lime powder is dissolved and emulsified into lime milk for standby.
The main reaction: caO+H 2 O→Ca(OH) 2
13 flocculant preparation
1) 1.5Kg of solid flocculant is weighed.
2) Opening a valve from the refined brine barrel (T-1181D) to a lime milk preparation barrel pipeline, automatically flowing refined brine to a flocculating agent preparation barrel (T-1185), or adding refined brine into the flocculating agent preparation barrel by a denitration calcium brine pump (P-1184A/B) when the liquid level of the refined brine barrel is low, and stopping adding refined brine when the liquid level reaches 2 meters; when the feed liquid reaches 1 meter, a stirring device (AG-1185) of the flocculant preparation barrel is started.
3) When refined bittern is added into the flocculant preparation barrel (T-1185) to the liquid level of 1.8 m, slowly adding the weighed solid flocculant into the flocculant preparation barrel (T-1185), and continuously stirring for 4 hours to dissolve the flocculant for later use.
1.4 calcium brine purification and pH adjustment
The calcium halide purification is to utilize hydroxide of lime dissolved in water and magnesium in the calcium halide to generate indissolvable magnesium hydroxide for removing magnesium, and the hydroxide generated by adding excessive lime is added to improve the pH of the calcium halide, and the main reaction formula is as follows: a) Lime hydrolysis: caO+H 2 O→Ca(OH) 2 The method comprises the steps of carrying out a first treatment on the surface of the B) Ionization of calcium hydroxide: ca (OH) 2 →Ca 2+ +2OH － The method comprises the steps of carrying out a first treatment on the surface of the C) Generating insoluble matters: 2OH － +Mg 2+ →Mg(OH) 2 And ∈. The specific operation is as follows:
1) When the feed liquid in the reaction barrel (T-1181B/C) reaches 16 meters, a lime milk pump is started to add the prepared lime milk into the reaction barrel (T-1181B/C), the lime milk pump is stopped according to the regulation after the lime milk conversion is completed, and a lime milk preparation barrel stirring device (AG-1184) is stopped.
2) When the feed liquid in the reaction barrel (T-1181B/C) reaches 19.5 m, the raw halogen pump is stopped, and the stirring device continuously stirs and reacts for 3 hours.
3) When the feed liquid in the reaction barrel (T-1181B/C) reaches 16 meters, a brine circulating pump (P-1188/1189) is started, and the pH value of the calcium brine is observed.
4) And taking a reaction barrel (T-1181B/C) calcium halide sample to detect the pH value of the calcium halide after stirring and reacting for 3 hours by an inspector.
5) When the pH value of the calcium halide is detected to reach 10.5, a flocculant pump is started to add the prepared flocculant into a reaction barrel (T-1181B/C), the flocculant pump is stopped according to the regulation after the flocculant is turned into materials, a flocculant preparation barrel stirring device (AG-1185) is stopped, and the reaction barrel stirring device (AG-1181B/C) continuously stirs for 5 minutes and then stops the stirring device (AG-1181B/C).
6) After the reaction barrel (T-1181B/C) is stopped and the stirring device is clarified for 3 hours, an inspector takes a calcium halide sample from the reaction barrel (T-1181B/C) to monitor NaCl and CaCl 2 Index such as pH value, solid, etc.
1.5 calcium brine storage and delivery
1) After monitoring that the reaction barrel (T-1181B/C) is clear and halogen-removing is qualified, a halogen-removing pump (P-1182) is started according to the regulations to transfer the clear halogen of the reaction barrel (T-1181B/C) to a refined halogen barrel (T-1181D).
2) And (3) starting a calcium halide conveying pump (P-1183A/B) according to a regulation to convey refined brine of a refined brine barrel (T-1181D) to a calcium halide barrel of a brine purifying workshop through a calcium halide pipe to serve as a raw material of a salt calcium production device.
1.6 reaction magnesium mud cleaning
1) After the halogen-removing material transferring of the reaction barrel (T-1181B/C) is completed, a stirring device (AG-1181B/C) is started to stir the magnesium mud to be in a suspension state.
2) After the magnesium mud is uniformly stirred, a mud pump (P-1185) is started according to the regulation to convey the mud of the reaction barrel (T-1181B/C) to a light calcium liquid barrel (T-1121B) through a mud pipe, and the mud is mixed with the light calcium liquid and then is injected into a well along with the light calcium liquid to produce brine.
Example 1 test results are shown in Table 2 below
TABLE 2
(1) Raw halogen (before pH adjustment): naCl is more than or equal to 270g/L, mgSO 4 0.2～0.3g/L、CaCl250g/L、pH 8.02。
2) Fine halogen control indexes: naCl is more than or equal to 270g/L, caCl, 50g/L, pH value is 10.5, solid content is less than or equal to 20ppm, and Mg 2+ Less than or equal to 6ppm or no.
As can be seen from Table 2, by the method of example 1, the pH was adjusted to 10.5 and the solid content was 20ppm or less, and Mg was not contained 2+ 。
Example 2
Example 2 differs from example 1 in that the room temperature is 30 c,
the weight formula of lime powder to be added for purifying and adjusting pH of calcium halide in each reaction barrel is as follows:
m (CaO) ＝C×(72447×c (Mg2+) +2784.11)×h÷ω (CaO)
wherein: m is m (CaO) Lime powder weight, unit/(Kg) is added for calcium halide purification and pH adjustment
c (Mg2+) -magnesium content in the calcium halide in units/(g/L)
h- - -reaction barrel (T-1181B/C) calcium halide level, unit/(m)
ω (CaO) Measuring the effective calcium oxide content of the lime powder, unit/(%)
And C, adding lime powder into the adjustment coefficient.
The C value is 1.00-1.05.
Other preparation methods and preparation conditions were identical to those of example 1.
Example 3
Example 3 differs from example 1 in that the room temperature is 10 c,
the weight formula of lime powder to be added for purifying and adjusting pH of calcium halide in each reaction barrel is as follows:
m (CaO) ＝C×(72447×c (Mg2+) +2784.11)×h÷ω (CaO)
wherein: m is m (CaO) Lime powder weight, unit/(Kg) is added for calcium halide purification and pH adjustment
c (Mg2+) -magnesium content in the calcium halide in units/(g/L)
h- - -reaction barrel (T-1181B/C) calcium halide level, unit/(m)
ω (CaO) Measuring the effective calcium oxide content of the lime powder, unit/(%)
And C, adding lime powder into the adjustment coefficient.
The C value is 1.00-1.05.
Other preparation methods and preparation conditions were identical to those of example 1.
Comparative example 1
Comparative example 1 differs from example 1 in that
The weight of lime powder is calculated according to the raw brine barrel, the calculated lime milk is directly added into a calcium brine raw brine barrel, then calcium brine enters a reaction barrel from the raw brine barrel, and flocculant is added, and other preparation methods and preparation conditions are consistent with those of the example 1.
Comparative example 2
Comparative example 2 differs from example 1 in that
The weight of lime powder is calculated according to the refined brine barrel, and the calculated lime milk and flocculant are directly added into the refined brine barrel, and other preparation methods and preparation conditions are the same as in example 1.
Examples 2-3 and comparative examples 1-2
The results of the measurements are shown in Table 3 below
TABLE 3 Table 3
As can be seen from Table 3, the weight of lime powder is increased by 1.02 times in examples 2 and 3 when the air temperature is higher or lower, so that the pH value can be ensured to reach 10.5; it can be seen from comparative example 1 that if the pH is adjusted by lime milk in the raw brine tank, the raw brine tank not only does not reach the standard, but also contains more solids, whereas from comparative example 2, the pH can reach the standard by directly adding lime milk in the refined brine tank, the pH value is higher, but the solid content is also higher; while examples 1-3 and comparative examples 1-2 control the Mg content well by adjusting the milk of lime.
The foregoing is only a preferred embodiment of the present application, but the scope of the present application is not limited thereto, and any person skilled in the art, who is within the scope of the present application, should be covered by the protection scope of the present application by equally replacing or changing the technical scheme and the inventive concept thereof.
Claims (5)
1. A method for purifying calcium halide, the method comprising the steps of:
s1, taking single-well calcium brine, and detecting the calcium brine, including detecting NaCl and CaCl 2 The method comprises the steps of carrying out a first treatment on the surface of the Introducing the calcium brine into a raw brine barrel, and detecting the calcium brine in the raw brine barrel, wherein the detection items comprise: naCl, caCl 2 、Mg 2＋ Content and pH value;
composition of the brine: naCl is more than or equal to 270g/L, mgSO 4 0.2~0.3 g/L、CaCl 2 50 g/L、pH 8.02；
S2, determining the weight of lime powder according to the data detected in the raw brine barrel in the step S1, and mixing the lime powder with refined brine to obtain lime milk;
the composition of the refined halogen comprises: naCl is more than or equal to 270g/L, caCl 2 50g/L, pH value of 10.5, solid content of less than or equal to 20ppm, mg 2 ＋ Less than or equal to 6ppm or no;
the method comprises the following steps:
s21, according to the liquid level of the calcium halide in the reaction barrel, mg 2＋ Calculating the weight of lime powder required by removing magnesium from calcium halide by the content and the CaO and MgO contents of the lime powder;
s22, calculating the weight of lime powder required by adjusting the pH value of the calcium halide according to the liquid level and the pH value of the calcium halide in the reaction barrel and the pH value adjusted to be not lower than 10.5; the sum of the weights of lime powder required by the calcium halide magnesium removal and the pH value adjustment is the weight of lime powder required by the calcium halide purification of the batch;
s23, calculating the weight of lime powder
The formula of the lime powder by weight is as follows:
m CaO =（230.73×c Mg2＋ ＋8.8666）×h÷ω CaO
wherein: m is m CaO Lime powder weight is added for purifying and regulating pH value of calcium halide, and the unit is per Kg
c Mg2＋ Magnesium content in calcium halide in units of g/L
V- - -reaction barrel T-1181B/C calcium halide volume, unit/m 3
ω CaO -measuring the effective calcium oxide content of the lime powder in units/%;
s3, mixing the calcium brine in the raw brine barrel in the step S1 with the lime milk obtained in the step S2 in a reaction barrel, and adding a flocculating agent after the reaction is completed;
the step S3 further comprises the following steps:
s4, after the clear and halogen-removing of the reaction barrel is detected to be qualified, the clear halogen in the reaction barrel is transferred to a refined halogen barrel;
s5, conveying clear brine in the fine brine barrel in the step S4 to a calcium brine barrel of a brine purifying workshop to serve as a raw material of a salt calcium production device;
and S1, the calcium halide is the calcium halide in the co-production of salt and calcium.
2. The method for purifying calcium halide according to claim 1, wherein the step S1 comprises the steps of:
s11, taking a single-well calcium halide sample, and analyzing and detecting NaCl and CaCl of each single-well calcium halide 2 ；
S12, feeding the calcium brine single-well brine into a calcium brine raw brine barrel, and calculating the total raw brine hour flow rate, wherein if the raw brine flow rate is more than 560 and 560m 3 /h; when the liquid level reaches 3 meters, starting the stirring device;
s13, if the flow rate of the raw halogen is lower than 560 and 560m 3 /h, caCl by calcium halide 2 And sodium nitrohalogenide Na 2 SO 4 Adding the difference of the supplementing calcium halogen amount;
s14, when the liquid level of the raw brine barrel reaches 14 meters, starting a raw brine pump to transfer materials to the reaction barrel, stopping transferring materials when the liquid level reaches 19.5 meters, and recording the liquid level of the reaction barrel; starting a stirring device matched with the reaction barrel when the feed liquid is 3 meters;
s15, taking a raw brine barrel calcium brine sample for analysis and detection of NaCl and CaCl of the calcium brine 2 pH value, mg 2＋ The content is as follows.
3. The method of claim 1, wherein the configuration of the milk of lime comprises the steps of:
s1, automatically flowing lime powder to a lime metering scale, and weighing the weight of the lime powder required by calcium halide purification;
s2, enabling refined brine to flow into a lime milk preparing barrel, adding lime powder into the lime milk preparing barrel, stirring, and continuously stirring to enable the lime powder to be dissolved and emulsified into lime milk for later use.
4. The method for purifying calcium halide according to claim 1, wherein the step S3 comprises the steps of:
s31, adding lime milk into the reaction barrel, and mixing and stirring with calcium halide in the reaction barrel;
s32, performing brine purification reaction;
s33, detecting the pH value of the calcium halide after stirring and reacting for 3 hours in a reaction barrel;
s34, if the pH value of the calcium halide is detected to be not lower than 10.5, adding the prepared flocculating agent into a reaction barrel, stopping a flocculating agent preparation barrel stirring device, and stopping stirring after the stirring device in the reaction barrel continuously stirs for 5 minutes;
s35, after the reaction barrel is clarified for 3 hours by stopping the stirring device, detecting calcium halide in the reaction barrel, wherein the detection items comprise: naCl, caCl 2 pH value and solid matter.
5. The method for purifying calcium halide as recited in claim 1, further comprising, after transferring the clear halide in the reaction tank to the refined halide tank:
s41, after the halogen clearing and material transferring of the reaction barrel are completed, stirring is started, and the reaction magnesium mud is stirred into a suspension state;
s42, after the reaction magnesium mud is uniformly stirred, conveying the mud to a light calcium liquid barrel, and injecting the light calcium liquid into a well to produce brine.
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