CN113247926A - Method for dissolving out calcium carbide slag instead of lime - Google Patents
Method for dissolving out calcium carbide slag instead of lime Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/06—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom by treating aluminous minerals or waste-like raw materials with alkali hydroxide, e.g. leaching of bauxite according to the Bayer process
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Abstract
A method for dissolving out by using carbide slag to replace lime relates to the technical field of chemical industry, and comprises the steps of mixing red mud and carbide slag for reaction to obtain activated carbide slag; then mixing the activated carbide slag and bauxite for dissolution. On one hand, the hydrated sodium aluminosilicate in the red mud can react with calcium hydroxide in the carbide slag to generate calcium hydrated garnet, and crystal water in the carbide slag is removed, so that the activity of the carbide slag is effectively improved, the carbide slag can perfectly replace lime when being applied to a dissolution link, and the same or even better dissolution effect is achieved. On the other hand, the red mud is waste generated in the process of producing alumina by the Bayer process, and when the red mud is used for activating the carbide slag, new impurities cannot be introduced, and the production control of oxidation is not influenced.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a method for dissolving out calcium carbide slag instead of lime.
Background
The carbide slag is calcium carbide (CaC) in the industrial production process of polyvinyl chloride (PVC), acetylene, polyvinyl alcohol, etc2) The main component of the industrial waste residue formed by hydrolysis is Ca (OH)2. China is the largest calcium carbide producing country and consuming country in the world, in 2016, the calcium carbide output in China reaches 2730 ten thousand tons, and each ton of calcium carbide generates 1.15-1.3 tons of calcium carbide slag after hydrolysis. Therefore, the discharge amount of the carbide slag exceeds 3000 ten thousand tons per year. The carbide slag is generally piled up, which occupies a large amount of land resources, and if the carbide slag is not processed in time, the carbide slag not only occupies the land resources, but also causes great pollution to the environment.
The main component of the carbide slag is calcium hydroxide, which generally accounts for 70-90% of the total mass, and in addition, the carbide slag also contains a small amount of inorganic and organic impurities (such as sulfide, phosphide, iron oxide, magnesium oxide, silicon dioxide and the like). It is grey white and has slight stink due to containing trace amount of carbon and sulfur and phosphorus impurities, and the long-time stacked aged slag also contains a small amount of calcium carbonate.
In the Bayer process for producing alumina, lime is needed in a plurality of links, such as a dissolution link of bauxite, a refining link of crude liquor by using a leaf filter, a causticization link of sodium carbonate by lime milk, a sodium removal link of red mud and the like, the main component of the lime is calcium oxide, and calcium hydroxide is also generated after the lime reacts with water, so in theory, the lime can be replaced by the carbide slag. If the production can be realized by replacing lime with the carbide slag, the lime loss is reduced, the production cost is reduced, a good channel is provided for recycling the carbide slag, and the production is more green and environment-friendly.
After a large number of creative experiments, the inventor of the invention finds that the carbide slag is used for replacing lime to assist in filtration in the leaf filter, the productivity and the head pressure of the leaf filter are influenced, and the purity of the filtered refined liquid is not influenced; the use of carbide slag instead of lime milk for causticizing sodium carbonate results in a significant reduction in causticization rate; the method has good effect of removing sodium from the red mud by replacing lime with carbide slag, and related achievements are already recorded in patent CN 201810059764.6; and the carbide slag is used for replacing lime for dissolution, and the dissolution rate is poor due to insufficient activity of the carbide slag.
Disclosure of Invention
The invention aims to provide a method for dissolving out carbide slag instead of lime, which is simple to operate and convenient to use, can effectively solve the problem of insufficient activity of the carbide slag in the process of dissolving out the carbide slag instead of the lime, obtains better dissolution rate and realizes the resource recycling of the carbide slag.
The embodiment of the invention is realized by the following steps:
a method for leaching by using carbide slag to replace lime, comprising the following steps:
mixing the red mud and the carbide slag for reaction to obtain activated carbide slag;
mixing the activated carbide slag and bauxite for dissolution.
The embodiment of the invention has the beneficial effects that:
the embodiment of the invention provides a method for dissolving out calcium carbide slag instead of lime, which comprises the steps of mixing red mud and the calcium carbide slag for reaction to obtain activated calcium carbide slag; then mixing the activated carbide slag and bauxite for dissolution. On one hand, the hydrated sodium aluminosilicate in the red mud can react with calcium hydroxide in the carbide slag to generate calcium hydrated garnet, and crystal water in the carbide slag is removed, so that the activity of the carbide slag is effectively improved, the carbide slag can perfectly replace lime when being applied to a dissolution link, and the same or even better dissolution effect is achieved. On the other hand, the red mud is waste generated in the process of producing alumina by the Bayer process, and when the red mud is used for activating the carbide slag, new impurities cannot be introduced, and the production control of oxidation is not influenced.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The following describes a method of dissolving out carbide slag instead of lime according to an embodiment of the present invention.
A method for leaching by using carbide slag to replace lime, comprising the following steps:
s1, mixing red mud and carbide slag for reaction to obtain activated carbide slag;
s2, mixing the activated carbide slag and bauxite for dissolution.
The inventors found that the effect of directly dissolving out the carbide slag instead of lime is very poor, and the carbide slag must be activated to achieve the desired effect. For this reason, the inventors tried to activate the carbide slag in various ways, including calcining, grinding, etc., and it was difficult to achieve the desired effect. The inventors have also attempted to activate the carbide slag by adding an active agent. Meanwhile, in order to avoid introducing new impurities, the most ideal activating agent is the material used or produced in the process of producing alumina by the Bayer process, the optional range comprises water, sodium aluminate solution, filter cake of leaf filter, red mud and the like, and finally the red mud is selected as the activating agent after multiple attempts and comparisons. On one hand, the red mud is waste generated in the process of producing alumina by a Bayer process, and when the red mud is used for activating the carbide slag, new impurities cannot be introduced, and the production control is facilitated. On the other hand, the inventor has studied another utilization mode of the carbide slag, namely a method for removing sodium from the red mud by using the carbide slag, wherein the method is to generate sodium hydroxide by using the reaction of calcium hydroxide in the carbide slag and hydrated sodium aluminosilicate in the red mud so as to achieve the purpose of removing the sodium. In this reaction, crystal water in the carbide slag is removed at the same time, and calcium garnet hydrate, that is, activated carbide slag, is produced. The specific equation is as follows:
Na2O·Al2O3·1.7SiO2·nH2O+nCa(OH)2→nCaO·Al2O3·xSiO2·(6-2x)H2O+2NaOH+nH2O
therefore, the activation of the carbide slag by the red mud is actually the comprehensive application of the carbide slag in two processes of sodium removal and dissolution, can recycle the carbide slag and the red mud simultaneously, and has more significance in environmental protection.
Wherein the carbide slag is waste slag generated in the production of polyvinyl chloride by using acetylene in a dry method, and the content of calcium hydroxide in the carbide slag is more than or equal to 85 wt%. It is worth noting that acetylene, if produced in a conventional manner, can typically produce calcium hydroxide in the carbide slag in amounts above 90 wt%.
The red mud is waste residue generated in the process of producing alumina by a Bayer process, the content of sodium oxide in the red mud is more than or equal to 4.5 wt%, and the sodium-silicon ratio (the mass ratio of sodium oxide to silicon oxide, which is abbreviated as N/S) is more than or equal to 0.4. Similarly, if alumina is produced in a conventional manner, the content of sodium oxide in the produced red mud can basically reach more than 5wt percent, and the requirement can be completely met.
Further, the mass ratio of the red mud to the carbide slag is 1: 1 to 3. The red mud is mixed according to the proportion, so that the activation effect of the red mud on the carbide slag is good, and the dissolution rate is improved. The temperature of the mixing reaction of the red mud and the carbide slag is 80-95 ℃, and the reaction time is 3-10 h. Under the reaction conditions, the carbide slag activating effect is better. After activation, the calcium-silicon ratio (mass ratio of calcium oxide to silicon oxide, abbreviated as C/S) in the obtained activated carbide slag is more than or equal to 4.5.
Further, when the digestion is carried out, the mass ratio of the bauxite to the activated carbide slag is 1: 0.15 to 0.25. During mixing, the activated carbide slag, bauxite and mother liquor are mixed together to prepare ore pulp for dissolution, and the content of the bauxite in the ore pulp is 0.25-0.3 g/ml. Within the above range, the dissolution effect is good, and the dissolution rate can reach or even exceed the result when lime is used.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The embodiment provides a method for dissolving out carbide slag instead of lime, which comprises the following steps:
s1, mixing 120g of red mud and 70g of carbide slag, and activating at 80 ℃ for 6 hours to obtain activated carbide slag;
s2, mixing 35.3g of activated carbide slag, 170g of bauxite and 620ml of mother liquor for dissolution.
The mass fractions of the main components of the red mud, the carbide slag, the bauxite, and the activated carbide slag used in the present example are shown in the following table (in the table, a/S is an aluminum-silicon ratio, that is, a mass ratio of alumina to silica).
| Sample name | Al2O3 | SiO2 | CaO | Ca(OH)2 | Na2O | A/S | C/S | N/S |
| Red mud | 18.50 | 11.01 | 21.30 | - | 5.20 | 1.68 | 1.93 | 0.47 |
| Carbide slag | 1.77 | 2.99 | - | 90.21 | - | 0.59 | - | - |
| Bauxite ore | 59.60 | 7.17 | 0.10 | - | - | 8.32 | 0.01 | - |
| Activated carbide slag | 12.68 | 8.75 | 47.15 | - | 1.10 | 1.45 | 5.39 | 0.13 |
Example 2
The embodiment provides a method for dissolving out carbide slag instead of lime, which comprises the following steps:
s1, mixing 120g of red mud and 100g of carbide slag, and activating at 80 ℃ for 10h to obtain activated carbide slag;
s2, mixing 29.6g of activated carbide slag, 170g of bauxite and 620ml of mother liquor for dissolution.
The mass fractions of the main components of the red mud, the carbide slag, and the activated carbide slag used in the present example are shown in the following table.
| Sample name | Al2O3 | SiO2 | CaO | Ca(OH)2 | Na2O | A/S | C/S | N/S |
| Red mud | 19.2 | 11.7 | 22.4 | - | 5.8 | 1.64 | 1.91 | 0.50 |
| Carbide slag | 1.73 | 2.94 | - | 92.2 | - | 0.59 | - | - |
| Bauxite ore | 59.60 | 7.17 | 0.10 | - | - | 8.32 | 0.01 | - |
| Activated carbide slag | 11.86 | 7.68 | 53.16 | - | 0.16 | 1.54 | 6.92 | 0.02 |
Example 3
The embodiment provides a method for dissolving out carbide slag instead of lime, which comprises the following steps:
s1, mixing 120g of red mud and 100g of carbide slag, and activating at 90 ℃ for 6 hours to obtain activated carbide slag;
s2, mixing 29.8g of activated carbide slag, 170g of bauxite and 620ml of mother liquor for dissolution.
The mass fractions of the main components of the red mud, the carbide slag, the bauxite, and the activated carbide slag used in the present example are shown in the following table.
| Sample name | Al2O3 | SiO2 | CaO | Ca(OH)2 | Na2O | A/S | C/S | N/S |
| Red mud | 17.4 | 10.6 | 21.6 | - | 5.6 | 1.64 | 2.04 | 0.53 |
| Carbide slag | 1.84 | 3.01 | - | 92.1 | - | 0.61 | - | - |
| Bauxite ore | 59.60 | 7.17 | 0.10 | - | - | 8.32 | 0.01 | - |
| Activated carbide slag | 12.07 | 8.13 | 53.32 | - | 0.46 | 1.48 | 6.56 | 0.06 |
Example 4
The embodiment provides a method for dissolving out carbide slag instead of lime, which comprises the following steps:
s1, mixing 120g of red mud and 70g of carbide slag, and activating at 90 ℃ for 10 hours to obtain activated carbide slag;
s2, mixing 35.7g of activated carbide slag, 170g of bauxite and 620ml of mother liquor for dissolution.
The mass fractions of the main components of the red mud, the carbide slag, the bauxite, and the activated carbide slag used in the present example are shown in the following table.
| Sample name | Al2O3 | SiO2 | CaO | Ca(OH)2 | Na2O | A/S | C/S | N/S |
| Red mud | 18.1 | 11.1 | 20.5 | - | 4.7 | 1.63 | 1.85 | 0.42 |
| Carbide slag | 1.71 | 2.9 | - | 91.4 | - | 0.59 | - | - |
| Bauxite ore | 59.60 | 7.17 | 0.10 | - | - | 8.32 | 0.01 | - |
| Activated carbide slag | 13.62 | 9.72 | 47.76 | - | 0.26 | 1.40 | 4.91 | 0.03 |
Comparative example 1
The present comparative example provides a method for leaching using carbide slag instead of lime, comprising:
s1, sintering the carbide slag at 800 ℃ for 10min to obtain activated carbide slag;
s2, mixing 35.3g of activated carbide slag, 170g of bauxite and 620ml of mother liquor for dissolution.
The compositions of the carbide slag and bauxite used in this comparative example were the same as in example 1.
Comparative example 2
The present comparative example provides a method for leaching using carbide slag instead of lime, comprising:
s1, grinding carbide slag into fine powder, and sieving the fine powder by using a 100-micron sieve to obtain activated carbide slag;
s2, mixing 35.3g of activated carbide slag, 170g of bauxite and 620ml of mother liquor for dissolution.
The compositions of the carbide slag and bauxite used in this comparative example were the same as in example 1.
Comparative example 3
This comparative example provides a process for digestion using carbide slag instead of lime, which operates in essentially the same manner as example 1, except that water is used as the activating agent instead of red mud to activate the carbide slag.
Comparative example 4
This comparative example provides a process for leaching out calcium carbide slag instead of lime, which operates in essentially the same manner as in example 1, except that the calcium carbide slag is activated with recycled mother liquor instead of red mud as the active agent.
Comparative example 5
This comparative example provides a process for digestion using carbide slag instead of lime, which operates in essentially the same manner as example 1, except that raw ore pulp is used as the activating agent instead of red mud to activate the carbide slag.
Comparative example 6
This comparative example provides a process for leaching out calcium carbide slag instead of lime, which operates in essentially the same manner as in example 1, except that the calcium carbide slag is activated with a leaf filter cake instead of red mud as an active agent.
Wherein the mass fraction of the main components of the filter cake of the leaf filter is as follows.
| Name (R) | Al2O3 | SiO2 | Fe2O3 | TiO2 | CaO | Na2O | A/S |
| Numerical value | 21.995 | 2.56 | 1.8475 | 0.20125 | 45.7025 | 0.375 | 9.35 |
Test example 1
The alumina is prepared by the traditional Bayer process, pure carbide slag, pure lime and carbide slag/lime mixture are respectively used for dissolution, red mud newly obtained after dissolution is detected, and the detection results are shown in Table 1.
TABLE 1 dissolution test data of carbide slag directly replacing part of lime
The bayer process elution effect can be seen from the magnitude of the aluminum-silicon ratio (a/S) in the obtained red mud, and a smaller value indicates a better elution effect. As can be seen from Table 1, the A/S ratio of the obtained red mud was 1.28 when the lime was used for leaching. And the A/S obtained by adopting pure carbide slag is 2.11, and compared with lime, the effect is obviously poor. However, it can be seen that the lime and the carbide slag are mixed at different ratios, and the dissolution effect is deteriorated as long as the carbide slag is added, and basically, the A/S is increased as the amount of the carbide slag is increased. From this, it is found that if the lime is entirely or partially replaced with the carbide slag as it is, the dissolution effect is deteriorated, and the intended purpose cannot be achieved.
Comparative example 2
The red mud newly obtained after dissolution in examples 1 to 4 and comparative examples 1 to 6 was subjected to a composition test, and the test results are shown in table 2.
TABLE 2 dissolution test data for activated carbide slag
| Sample name | Al2O3 | SiO2 | CaO | Na2O | A/S | Dissolution rate/%) |
| Bauxite ore | 59.60 | 7.17 | 0.10 | - | 8.32 | - |
| Lime leaching | 18.03 | 13.23 | 12.50 | 6.22 | 1.36 | 83.65 |
| Example 1 | 17.48 | 12.66 | 14.37 | 4.87 | 1.38 | 83.41 |
| Example 2 | 17.14 | 12.84 | 13.97 | 5.05 | 1.33 | 84.01 |
| Example 3 | 17.65 | 12.89 | 12.68 | 5.44 | 1.37 | 83.53 |
| Example 4 | 16.94 | 12.81 | 14.23 | 4.92 | 1.32 | 84.13 |
| Comparative example 1 | 24.8 | 13.03 | 15.40 | 5.90 | 1.90 | 77.12 |
| Comparative example 2 | 28.12 | 9.27 | 7.80 | 5.95 | 3.03 | 63.54 |
| Comparative example 3 | 35.6 | 7.8 | 8.10 | 5.40 | 4.56 | 45.14 |
| Comparative example 4 | 26.7 | 13.7 | 12.8 | 7.3 | 1.95 | 76.58 |
| Comparative example 5 | 26.9 | 13.59 | 12.8 | 7.7 | 1.98 | 76.21 |
| Comparative example 6 | 33.8 | 9.8 | 15 | 5.2 | 3.45 | 58.55 |
As can be seen from Table 2, the dissolution rate of lime in the conventional dissolution process reaches 83.65%, but the dissolution rate of the method of the embodiments 1 to 4 of the present invention, which is replaced by carbide slag, is 83.41 to 84.13%, which is equivalent to or slightly beyond the effect of lime dissolution. In contrast, the dissolution rate is reduced by 5-40% through high-temperature sintering activation (comparative example 1), grinding activation (comparative example 2) or activation of other active agents (comparative examples 3-6), and the condition of replacing lime is obviously not met. It should be noted that in the case of the high-temperature sintering of the comparative example, in the actual test process, the leaching effect is very unstable, the measured result is sometimes poor and sometimes even better than that of lime leaching, and the high-temperature sintering is not recommended to be used for activation in consideration of the large energy loss caused by the high temperature. Note that the above dissolution rate is calculated as follows.
Dissolution rate (A/S of red mud obtained from A/S-of bauxite)/(A/S of bauxite)
Qualitatively, the larger the A/S of the obtained red mud, the lower the dissolution rate.
Test example 3
The method for dissolving out by using carbide slag to replace lime provided by the embodiment of the invention is actually operated in an aluminum production factory where the inventor is located, and according to the scale of the factory, only a dissolving-out link is needed every year, so that about 40 ten thousand tons of lime is consumed. The polyvinyl chloride manufacturer who works with the plant produces about 15 ten thousand tons of carbide slag every year, and the amount of carbide slag is converted into about 11.25 ten thousand tons of lime on the basis of the calcium content. By adopting the method provided by the embodiment of the invention, the carbide slag is completely digested, about 28% of lime loss of the plant is saved, and the method not only brings huge economic value, but also has great significance for environmental protection.
In summary, the embodiment of the present invention provides a method for dissolving out calcium carbide slag instead of lime, which includes mixing red mud and calcium carbide slag for reaction to obtain activated calcium carbide slag; then mixing the activated carbide slag and bauxite for dissolution. On one hand, the hydrated sodium aluminosilicate in the red mud can react with calcium hydroxide in the carbide slag to generate calcium hydrated garnet and remove crystal water in the carbide slag, so that the activity of the carbide slag is effectively improved, the carbide slag can perfectly replace lime when being applied to a dissolution link, and the same or even better dissolution effect is achieved. On the other hand, the red mud is waste generated in the process of producing alumina by the Bayer process, and when the red mud is used for activating the carbide slag, new impurities cannot be introduced, a channel is provided for the waste treatment and reutilization of the red mud, and the red mud is more green and environment-friendly.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A method for dissolving out lime replaced by carbide slag is characterized by comprising the following steps:
mixing the red mud and the carbide slag for reaction to obtain activated carbide slag;
and mixing the activated carbide slag and bauxite for dissolution.
2. The method according to claim 1, wherein the mass ratio of the red mud to the carbide slag is 1: 1 to 3.
3. The method for leaching by using the carbide slag to replace lime according to claim 2, wherein the temperature of the mixing reaction of the red mud and the carbide slag is 80-95 ℃ and the reaction time is 3-10 h.
4. The method for leaching by using carbide slag to replace lime according to claim 3, wherein the calcium-silicon ratio in the activated carbide slag is not less than 4.5.
5. The method for leaching by using carbide slag instead of lime according to claim 1, wherein the mass ratio of the bauxite to the activated carbide slag is 1: 0.15 to 0.25.
6. The method for leaching by using carbide slag to replace lime according to claim 5, wherein the activated carbide slag and the bauxite are prepared into pulp, and the content of the bauxite in the pulp is 0.25-0.3 g/ml.
7. The method for dissolving out the calcium carbide slag instead of the lime according to claim 1, wherein the calcium carbide slag is waste slag generated in the production of polyvinyl chloride by using acetylene in a dry method, and the content of calcium hydroxide in the calcium carbide slag is not less than 85 wt%.
8. The method for dissolving out by using carbide slag to replace lime according to claim 1, wherein the red mud is waste slag generated in the process of producing alumina by a Bayer process, the content of sodium oxide in the red mud is not less than 4.5 wt%, and the sodium-silicon ratio is not less than 0.4.
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