CN115108738A - Calcium hydroxide suspension and preparation method thereof - Google Patents
Calcium hydroxide suspension and preparation method thereof Download PDFInfo
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- CN115108738A CN115108738A CN202210709279.5A CN202210709279A CN115108738A CN 115108738 A CN115108738 A CN 115108738A CN 202210709279 A CN202210709279 A CN 202210709279A CN 115108738 A CN115108738 A CN 115108738A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2/00—Lime, magnesia or dolomite
- C04B2/02—Lime
- C04B2/04—Slaking
- C04B2/06—Slaking with addition of substances, e.g. hydrophobic agents ; Slaking in the presence of other compounds
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Abstract
The invention discloses a calcium hydroxide suspension and a preparation method thereof, which comprises the steps of crushing and sieving quicklime, adding slaking water into a reactor with a stirring device, wherein the mass ratio of the slaking water to the standby quicklime is 2: 1-4: 1, adding an active promoter and/or a stabilizer dissolved in the slaking water, adding the quicklime into the reactor under the state of continuous stirring of the stirring device, wherein the time of the adding process is not more than 15min, the reaction time of the slaking reaction temperature higher than 60 ℃ is not more than 60min and not less than 10min in the slaking reaction process, and after the slaking reaction is finished, carrying out hydrocyclone separation and/or screening on a product mixed solution in the reactor to remove large-particle impurities in the mixed solution, thereby obtaining a target calcium hydroxide suspension finished product. The invention can obtain the calcium hydroxide suspension with high reaction activity, high calcium hydroxide content and low viscosity by accurately controlling the raw materials, the process and the auxiliary agent, and has the advantages of simple process, high efficiency and low cost.
Description
Technical Field
The invention belongs to the technical field of calcium hydroxide production, and relates to a calcium hydroxide suspension and a preparation method thereof.
Background
The calcium hydroxide is widely applied in the water treatment fields of neutralization of acidic wastewater, removal of heavy metal ions, phosphate ions, sulfate ions, fluoride ions and the like. In water treatment practice, calcium hydroxide is generally used as a suspension with water or after a calcium hydroxide suspension is obtained by wet digestion of calcium oxide.
The calcium hydroxide has the advantages of good safety and lower price than inorganic alkaline treatment agents such as sodium hydroxide, sodium carbonate and the like, but the defects mainly comprise two aspects: firstly, calcium hydroxide is slightly soluble in water, and compared with water-soluble alkali such as sodium hydroxide and the like, when a chemical reaction occurs, the calcium hydroxide is firstly dissolved in water, and then calcium ions or hydroxyl ions react with harmful substances in wastewater, so that the treatment speed of the calcium hydroxide is slower than that of the water-soluble alkali such as sodium hydroxide and the like when the calcium hydroxide is used for treating the wastewater, and the efficiency of water treatment is influenced; secondly, the solid content of the common calcium hydroxide suspension is 5-10% (while the concentration of the sodium hydroxide solution commonly used for water treatment is more than 30%), and the viscosity of the suspension is too high due to the high concentration, so that the suspension is difficult to convey and measure, and the production load and the production cost in the pulp preparation link are obviously increased. In addition to the two main defects, calcium hydroxide also has the problems of incomplete reaction, excessive addition, high impurity content, increased water treatment sludge amount and the like. Therefore, from the application point of view, calcium hydroxide suspension with high reactivity, high solid content, low viscosity and low impurity content is ideal for the water treatment industry.
It has been found that the dissolution rate of calcium hydroxide in water is related to the particle size, the smaller the particle size, the faster the dissolution rate, and correspondingly the faster the chemical reaction rate, the better the reactivity of calcium hydroxide. At the same time, however, the smaller the particle size, the greater the viscosity of the suspension, which limits the increase in the calcium hydroxide content of the suspension. Therefore, it is technically difficult to obtain a calcium hydroxide suspension having high reactivity, high content and low viscosity at the same time.
To solve the above problems, a great deal of research has been conducted, which mainly includes:
1. the viscosity of the suspension is reduced by using an additive which can form precipitates or slightly soluble substances with calcium ions, for example, when calcium oxide is subjected to a digestion reaction with water, substances such as gypsum and the like are added into the water to reduce the viscosity of lime milk. However, this method causes a decrease in the reactivity of calcium hydroxide.
2. During the preparation of calcium hydroxide suspension or during the wet digestion of calcium oxide, organic polymer dispersant is added to reduce viscosity, for example, polyacrylate dispersant is added in patent W02018/048633A1 to reduce viscosity of calcium hydroxide suspension. Although the addition of the dispersant can reduce the viscosity of the suspension, the primary particle size of the calcium hydroxide cannot be reduced, i.e., the reactivity of the calcium hydroxide is not improved.
3. The method of wet milling (or milling plus dispersing agent) is used to reduce the particle size of the calcium hydroxide and thereby increase the reactivity of the calcium hydroxide, as disclosed in US 2019002301. The method increases the preparation steps of the suspension, is more complicated, and increases the addition proportion of corresponding additives although the particle size is reduced, thereby bringing obvious influence on the production cost.
4. High activity, low viscosity suspensions were prepared by varying the digestion process. For example, in patents CN106470960 and US2019092684, suspensions of calcium hydroxide are prepared by stepwise addition of water to lime, the water containing a dispersant or an inorganic salt. This approach is highly desirable for digestion equipment because at low water-to-cement ratios the lime digest is pasty and has an extremely high viscosity that ordinary equipment cannot meet.
In summary, the above methods are all pursuing a certain property of the calcium hydroxide suspension, and affect other properties of the suspension, so that the methods for preparing the calcium hydroxide suspension in the prior art have many disadvantages, which causes the prior art to fail to produce the calcium hydroxide suspension with high reactivity, high solid content, low viscosity and low impurity content, and limits the industrial application and development of the calcium hydroxide suspension.
Disclosure of Invention
In order to fill the blank of the prior art, the invention provides a calcium hydroxide suspension with high reactivity, high calcium hydroxide content and low viscosity and a preparation method thereof, so as to overcome the defects of the prior art.
The technical scheme of the invention is as follows:
a preparation method of calcium hydroxide suspension comprises the following steps:
s1: crushing and sieving quicklime with activity degree not lower than 360, screening quicklime with particle size smaller than 8mm, and weighing for later use;
s2: adding slaking water into a reactor with a stirring device, wherein the mass ratio of the slaking water to the standby quicklime is 2: 1-4: 1, the water temperature is controlled at 15-40 ℃, an active promoter and/or a stabilizer are added and dissolved into the slaking water, the ratio of the total added mass of the active promoter and/or the stabilizer to the mass of the standby quicklime is 5: 1000-40: 1000, the active promoter is a substance which can make water alkaline after being dissolved in water and is mixed with calcium hydroxide to avoid generating precipitates, and the stabilizer is one or a mixture of micromolecular dispersant, sugar alcohol and saccharide;
s3: adding the standby quicklime into a reactor under the state of continuous stirring by a stirring device, wherein the adding process ensures that the quicklime and the water for digestion are uniformly mixed, and the quicklime is not accumulated in the reactor, on the basis, the time of the adding process is not more than 15min, and in the digestion reaction process, the reaction time of the reactant with the temperature higher than 60 ℃ is not more than 60min and not less than 10 min;
s4: and after the digestion reaction is finished, carrying out hydrocyclone separation and/or screening on the product mixed liquor in the reactor to remove large-particle impurities in the product mixed liquor so as to obtain a finished product of the target calcium hydroxide suspension.
Further, in the S1, the particle size of the standby quicklime is less than 5 mm.
Further, in the step S1, the activity of quicklime is not lower than 380.
Further, in the step S3, the time length of the feeding process does not exceed 10 min.
Further, in the step S3, the time period of the feeding process does not exceed 5 min.
Further, the activity promoter is one or a mixture of more of sodium hydroxide, potassium hydroxide, sodium acetate, sodium formate, monoethanolamine, diethanolamine and triethanolamine.
Further, the stabilizer is one or a mixture of potassium pyrophosphate, sodium hexametaphosphate, xylitol, sorbitol, erythritol, sucrose, glucose and fructose.
Furthermore, the ratio of the total mass of the added active accelerant and/or stabilizer to the mass of the ready quicklime is 10: 1000-30: 1000.
The calcium hydroxide suspension prepared by any one of the preparation methods comprises 2545% of calcium hydroxide by mass, 3 mu m-D50-5.5 mu m in particle size distribution, D97-20 mu m, D100-40 mu m, 450 centipoises at 25 ℃ and t 90-4 seconds of reaction activity.
The activity of the quicklime mentioned in step S1 is tested according to the method specified in YB/T105-. The method has the advantages that the quicklime is crushed and then used, so that the digestion reaction process is more uniform and stable, the phenomena of bumping, local overheating and the like caused by porous massive lime are reduced, and the stability of the product quality is facilitated. The size of the ground and sieved lime particles is not more than 8mm, otherwise the phenomena of bumping and the like are easily caused; the size of the crushed and sieved quicklime particles is preferably less than 5mm, and experiments show that the size has more remarkable effect on eliminating phenomena such as bumping and the like.
In step S2, the water temperature of the digestion water is lower than 15 ℃ resulting in a decrease in the reactivity of the resulting calcium hydroxide suspension, while higher than 40 ℃ resulting in a significant increase in the viscosity of the calcium hydroxide suspension. The mentioned active promoter is a substance which can make water alkaline after being dissolved in water, but does not include a substance which can react with calcium hydroxide to generate precipitate, and sodium hydroxide, potassium hydroxide, sodium acetate, sodium formate, monoethanolamine, diethanolamine, triethanolamine and the like are preferred. The mentioned stabilizer has double functions of improving the reaction activity of calcium hydroxide and reducing the agglomeration of calcium hydroxide particles, can be used alone or together with an activity promoter, and preferred stabilizers include small molecular dispersing agents such as potassium pyrophosphate, sodium hexametaphosphate, sugar alcohols such as xylitol, sorbitol, erythritol and sugar substances such as sucrose, glucose, fructose and the like. The total mass of the active promoter and/or stabilizer added is 0.5-4%, preferably 1-3% of the mass of the active quicklime.
In step S3, the slow feeding speed of the quicklime affects the production efficiency on the one hand, and on the other hand, the slow feeding speed of the quicklime causes the reduction of the reaction activity of the product and the increase of the viscosity, so the feeding time of the quicklime does not exceed 15 minutes, and is preferably controlled within 10 minutes or 5 minutes, but the feeding is not too fast, and the quicklime and the water are uniformly mixed and the quicklime is not accumulated in the reactor during feeding. When calcium hydroxide is generated through the digestion reaction of quicklime and water, heat is released to cause the temperature of a reaction system to rise, for the preparation of a calcium hydroxide suspension, the temperature rise is beneficial to more complete digestion reaction, but the reaction activity of the calcium hydroxide is reduced due to long-time high temperature, and the digestion reaction is incomplete due to short high temperature time, so that the time of the digestion reaction temperature of over 60 ℃ is not more than 60 minutes and not less than 10 minutes. The mass ratio of the water for the digestion reaction to the quicklime is 2: 1-4: 1, the viscosity is too high when the water-lime ratio is too low, and the content of calcium hydroxide in the suspension is low when the water-lime ratio is too high, so that the economy is not good.
In step S4, the suspension obtained after the digestion reaction is removed of large particles by means of a hydrocyclone and/or a vibrating screen, which can remove the unreacted impurities carried in the lime raw material, such as silica, alumina, and unburnt limestone, to increase the content of calcium hydroxide in the suspension and reduce the amount of sludge generated during sewage treatment.
In conclusion, the beneficial effects of the invention are as follows:
the invention prepares the calcium hydroxide suspension with high reactivity, high calcium hydroxide content and low viscosity by accurately controlling the raw materials, the process and the auxiliary agent, overcomes the technical problem that the calcium hydroxide suspension with high reactivity, high calcium hydroxide content and low viscosity cannot be prepared in the prior art, can remove most impurities in the suspension by a hydrocyclone separation or sieving method, and solves the problems of low reaction speed, low production efficiency, high addition amount, more sludge and the like existing in the prior calcium hydroxide in water treatment application.
The invention does not use expensive polymer dispersant, the used additives are common small molecular chemical reagents, and the optimal effect is realized by the combination of different reagents; meanwhile, the invention does not need special equipment (such as a high-torque digester and the like), has simple operation and short reaction flow, and is favorable for reducing the manufacturing cost of the suspension.
Detailed Description
The following describes in detail embodiments of the present invention.
The process flow for preparing the calcium hydroxide suspension comprises the following four steps:
s1: crushing and sieving quicklime with activity degree not lower than 360, screening quicklime with particle size smaller than 8mm, and weighing for later use;
s2: adding water for digestion into a reactor with a stirring device, wherein the mass ratio of the water for digestion to the standby quicklime is 2: 1-4: 1, the water temperature is controlled at 15-40 ℃, an active promoter and/or a stabilizer are dissolved in the water for digestion, the ratio of the total mass of the active promoter and/or the stabilizer to the mass of the standby quicklime is 5: 1000-40: 1000, the active promoter is a substance which can make the water alkaline after being dissolved in the water and is mixed with the calcium hydroxide to avoid generating precipitates, and the stabilizer is one or a mixture of micromolecular dispersant, sugar alcohol and saccharide;
s3: adding the standby quicklime into a reactor under the state of continuous stirring by a stirring device, wherein the adding process ensures that the quicklime and the water for digestion are uniformly mixed, and the quicklime is not accumulated in the reactor, on the basis, the time of the adding process is not more than 15min, and in the digestion reaction process, the reaction time of the reactant with the temperature higher than 60 ℃ is not more than 60min and not less than 10 min;
s4: and after the digestion reaction is finished, carrying out hydrocyclone separation and/or screening on the product mixed liquor in the reactor to remove large-particle impurities in the product mixed liquor so as to obtain a finished product of the target calcium hydroxide suspension.
Example 1
10kg of slaking water having a temperature of 40 ℃ and containing 10g of sodium hydroxide and 10g of potassium pyrophosphate dissolved therein was charged into a stirred reactor, and 2.5kg of quicklime powder having an activity of 400 (particle size < 5mm, added over 15 minutes) was added to the water under stirring. And (3) after adding the quicklime, quickly heating the reaction system, continuously stirring for 60 minutes after the temperature exceeds 60 ℃, stopping stirring, discharging the suspension from the reaction kettle, and sieving by a 200-mesh sieve to obtain a finished calcium hydroxide suspension.
The calcium hydroxide suspension obtained, in which the content of calcium hydroxide was measured according to the method specified in GB/T278152011 "Industrial milk calcium hydroxide"; the viscosity of the suspension is tested by using an NDJ-9S rotational viscometer, the temperature of the suspension is stabilized at 25 ℃, and the suspension is tested by using a No. 2 or No. 3 rotor at the rotating speed of 60 revolutions per minute; the particle size distribution of the solid particles in the suspension was tested using a laser particle sizer; the reactivity of the calcium hydroxide in the suspension was determined by conductivity method, i.e. according to the calcium hydroxide content of the suspension, 0.1g of the suspension containing calcium hydroxide was weighed, poured quickly into 700g of deionized water (water temperature 25 ℃) while recording the change of the conductivity of the deionized water with time, and the time elapsed from the pouring of the calcium hydroxide suspension until the conductivity reached 90% of the maximum value was calculated and recorded as t 90. A smaller t90 indicates a higher dissolution rate of calcium hydroxide and higher reactivity.
Tests show that the calcium hydroxide suspension prepared in the embodiment has the following indexes: the calcium hydroxide content was 25%, t90 ═ 4 seconds, viscosity 182cP, D50 ═ 5.5 μm, D97 ═ 17.8 μm, and D100 ═ 40 μm.
Example 2
9kg of digestion water at 15 ℃ in which 20g of sodium acetate and 90g of glucose were dissolved was charged into a stirred reactor, and 4.5kg of quicklime powder having an activity of 360 (particle size < 8mm, added over 5 minutes) was added to the water under stirring. After the quicklime is added, the reaction system is rapidly heated, stirring is continuously carried out for 10 minutes after the temperature exceeds 60 ℃, then stirring is stopped, the suspension is discharged from the reaction kettle and sieved by a 200-mesh sieve, and the calcium hydroxide suspension with the calcium hydroxide content of 45 percent, the t90 of 2.4 seconds, the viscosity of 450cP, the D50 of 3 μm, the D97 of 14.9 μm and the D100 of 33.5 μm is obtained.
Example 3
9kg of digestion water having a temperature of 20 ℃ and containing 60g of sorbitol and 30g of sodium hexametaphosphate dissolved therein was charged into a stirred reactor, and 3kg of quicklime powder having an activity of 380 (particle size < 5mm, added over 10 minutes) was added to the water under stirring. After the quicklime is added, the reaction system is rapidly heated, after the temperature exceeds 60 ℃, stirring is continuously carried out for 40 minutes, then stirring is stopped, the suspension is discharged from the reaction kettle and sieved by a 200-mesh sieve, and the calcium hydroxide suspension with the calcium hydroxide content of 35 percent, the t90 is 3.2 seconds, the viscosity of 356cP, the D50 is 5 micrometers, the D97 is 20 micrometers and the D100 is 40 micrometers is obtained.
Example 4
10kg of digestion water having a temperature of 30 ℃ and containing 25g of triethanolamine, 25g of xylitol and 50g of sucrose was charged into a stirred reactor, and 2.5kg of quicklime powder having an activity of 390 (particle size < 5mm, added within 5 minutes) was added to the water under stirring. After the quicklime is added, the reaction system is rapidly heated, stirring is continuously carried out for 30 minutes after the temperature exceeds 60 ℃, then stirring is stopped, the suspension is discharged from the reaction kettle and sieved by a 200-mesh sieve, and the calcium hydroxide suspension with the calcium hydroxide content of 25%, t90 ═ 3.5 seconds, the viscosity of 203cP, D50 ═ 4.8 μm, D97 ═ 16.2 μm and D100 ═ 38.7 μm is obtained.
Through repeated experiments of continuous control variables, the content of calcium hydroxide in the prepared calcium hydroxide suspension is 25-45%, the particle size distribution is that D50 is more than or equal to 3 mu m and less than or equal to 5.5 mu m, D97 is more than or equal to 20 mu m, D100 is more than or equal to 40 mu m, the viscosity is less than or equal to 450 centipoises (namely cP, 1cP is 1mPa.s) at 25 ℃, and the reaction activity t90 is less than or equal to 4 seconds.
With the above examples, the calcium hydroxide suspension prepared by the method of the present invention has a calcium hydroxide mass content of 25-45%, a particle size distribution of 3 μm or more and D50 or less and 5.5 μm or less, D97 or less and 20 μm or less, D100 or less and 40 μm or less, a viscosity at 25 ℃ or less of 450 centipoise (centipoise cP, 1cP being 1mpa.s) or less, and a reactivity t90 or less of 4 seconds.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. The present invention is not limited to the above-described embodiments, which are described in the specification and illustrated only for illustrating the principle of the present invention, but various changes and modifications may be made within the scope of the present invention as claimed without departing from the spirit and scope of the present invention. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. A method for preparing calcium hydroxide suspension is characterized in that: the method comprises the following steps:
s1: crushing and sieving quicklime with activity degree not lower than 360 to screen quicklime with particle size less than 8mm, and weighing for later use;
s2: adding water for digestion into a reactor with a stirring device, wherein the mass ratio of the water for digestion to the standby quicklime is 2: 1-4: 1, the water temperature is controlled at 15-40 ℃, an active promoter and/or a stabilizer are dissolved in the water for digestion, the ratio of the total mass of the active promoter and/or the stabilizer to the mass of the standby quicklime is 5: 1000-40: 1000, the active promoter is a substance which can make the water alkaline after being dissolved in the water and is mixed with the calcium hydroxide to avoid generating precipitates, and the stabilizer is one or a mixture of micromolecular dispersant, sugar alcohol and saccharide;
s3: adding the standby quicklime into a reactor under the state of continuous stirring by a stirring device, wherein the adding process ensures that the quicklime and the water for digestion are uniformly mixed, and the quicklime is not accumulated in the reactor, on the basis, the time of the adding process is not more than 15min, and in the digestion reaction process, the reaction time of the reactant with the temperature higher than 60 ℃ is not more than 60min and not less than 10 min;
s4: and after the digestion reaction is finished, carrying out hydrocyclone separation and/or screening on the product mixed liquor in the reactor to remove large-particle impurities in the product mixed liquor so as to obtain a finished product of the target calcium hydroxide suspension.
2. The method of preparing a calcium hydroxide suspension according to claim 1, wherein: in the S1, the particle size of the spare quicklime particles is less than 5 mm.
3. The method of preparing a calcium hydroxide suspension according to claim 1, wherein: in the S1, the activity of the quicklime is not lower than 380.
4. The method of preparing a calcium hydroxide suspension according to claim 1, wherein: in the S3, the time length of the feeding process does not exceed 10 min.
5. The process for preparing a calcium hydroxide suspension according to claim 1 or 4, wherein: in the S3, the time of the feeding process does not exceed 5 min.
6. The method of preparing a calcium hydroxide suspension according to claim 1, wherein: the activity promoter is one or a mixture of more of sodium hydroxide, potassium hydroxide, sodium acetate, sodium formate, monoethanolamine, diethanolamine and triethanolamine.
7. The method of preparing a calcium hydroxide suspension according to claim 1, wherein: the stabilizer is one or more of potassium pyrophosphate, sodium hexametaphosphate, xylitol, sorbitol, erythritol, sucrose, glucose and fructose.
8. The method of preparing a calcium hydroxide suspension according to claim 1, wherein: the ratio of the total mass of the active accelerant and/or the stabilizer to the mass of the standby quicklime is 10: 1000-30: 1000.
9. A calcium hydroxide suspension characterized by: the calcium hydroxide suspension prepared by any one of the preparation methods has the calcium hydroxide content of 25-45% by mass, the particle size distribution of D50 which is more than or equal to 3 mu m and less than or equal to 5.5 mu m, D97 which is less than or equal to 20 mu m, D100 which is less than or equal to 40 mu m, the viscosity at 25 ℃ which is less than or equal to 450 centipoises, and the reaction activity t90 which is less than or equal to 4 seconds.
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| CN112358205A (en) * | 2020-11-27 | 2021-02-12 | 广西合山市华纳新材料科技有限公司 | Preparation method of high-activity calcium hydroxide |
| CN114522554A (en) * | 2022-02-20 | 2022-05-24 | 深圳市长隆科技有限公司 | Preparation and application of superfine suspended calcium hydroxide |
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| JPH09268011A (en) * | 1996-03-29 | 1997-10-14 | Okutama Kogyo Kk | Aqueous suspension of high concentration calcium hydroxide |
| JP2010180086A (en) * | 2009-02-04 | 2010-08-19 | Yoshizawa Lime Industry | Method for producing slaked lime |
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| CN114522554A (en) * | 2022-02-20 | 2022-05-24 | 深圳市长隆科技有限公司 | Preparation and application of superfine suspended calcium hydroxide |
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