CN1268487A - Treatment and utilization method of waste acid liquor by using activated clay - Google Patents
Treatment and utilization method of waste acid liquor by using activated clay Download PDFInfo
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- CN1268487A CN1268487A CN 00112223 CN00112223A CN1268487A CN 1268487 A CN1268487 A CN 1268487A CN 00112223 CN00112223 CN 00112223 CN 00112223 A CN00112223 A CN 00112223A CN 1268487 A CN1268487 A CN 1268487A
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Abstract
A treatment and utilization method of activated clay waste acid is disclosed. It is that water glass is added to the waste acid produced during the manufacture of activated clay, through mixing thoroughly to react, separating out the precipitate after reaction, washing with water, drying, and grinding to obtain the precipitated mixture product. The mother liquid contains only sodium salt of strong inorganic acid and neutral liquid of sodium silicate. The present invention is simple in treatment process, low in treatment cost, and the output precipitated mixture has relatively great usage value without residue produced.
Description
The invention relates toa method for treating and utilizing waste liquid, in particular to a method for treating and utilizing waste acid liquid generated by manufacturing activated clay by using wet-process strong-acid inorganic acid activated aluminosilicate clay minerals.
In the prior art, the waste acid liquor generated by manufacturing activated clay by using wet method strong acid inorganic acid to activate aluminosilicate clay mineral, such as activated clay manufactured by activating natural bentonite mineral with strong acid inorganic acid, also called activated bleaching clay, has the by-product strong acid waste acid liquor of 35-60 meters which needs to be discharged when producing one ton of high-efficiency activated clay3. The main chemical substances of these waste acid solutions mainly include free strong acid inorganic acid and small amount of aqueous solutions of aluminum salt, magnesium salt and calcium salt of strong acid inorganic acid, such as aqueous solutions of sulfuric acid, aluminum sulfate, magnesium sulfate, calcium sulfate, nitric acid, aluminum nitrate, magnesium nitrate, calcium nitrate, hydrochloric acid, aluminum chloride, magnesium chloride and calcium chloride, because these waste acid solutions have a dilute concentration of strong acid inorganic acid and contain many impurities of strong acid inorganic salt, they are highly corrosive and have a large amount to be treated, so that they are difficult to be comprehensively utilized. The treatment method disclosed in the prior art is to discharge the lime or limestone after neutralization, the treatment process is very complicated, the treatment cost is very high and reaches about 100 percent of the production cost, and the product with high use value cannot be recycled. The discharged neutral waste water also contains a plurality of water-soluble inorganic acid salts, which still causes certain pollution, and the amount of the generated waste residue cake reaches about 80 percent of the product yield.
The invention aims to provide a method for treating and utilizing activated clay pickle liquor, aiming at the defects of the prior art.
The invention aims to achieve the purpose by the following technical scheme, and the invention discloses a method for treating and utilizing activated clay pickle liquor, which is characterized by comprising the following steps of: sampling and analyzing the waste acid liquor produced by using wet-process strong acid inorganic acid to activate aluminosilicate clay mineral to make activated clay, measuring out effective content of its strong acid inorganic acid, adding sodium silicate Na as effective component according to the weight ratio of 1: 3.0-7.2 of effective content2SiO3]The water glass is fully stirred and reacted with strong acid inorganic acid in waste acid liquor and aluminum salt, magnesium salt and calcium salt of the strong acid inorganic acid at the temperature of 20-100 ℃, and the reaction is carried outSilicic acid [ H]formed in the post-feed liquid2SiO3↓]Aluminum silicate [ Al2(SiO3)3↓]Calcium silicate [ CaSiO]3↓]Magnesium silicate [ MgSiO]3↓]Separating out precipitate, washing with water, drying at 105-200 deg.C, dewatering, and grinding to obtain precipitate mixture product, whose mother liquor only contains strong acid inorganic acid sodium salt and small amount of excessive sodium silicate [ Na]2SiO3]To a neutral aqueous solution of (a).
In the above process, the strongly acidic inorganic acid mainly means sulfuric acid, hydrochloric acid and nitric acid or a mixed acid of these acids. The chemical component of the water glass is sodium silicate Na2SiO3·nH2O, the sodium silicate and the strong acid inorganic acid in the waste acid liquor and the aluminum salt, the magnesium salt and the calcium salt of the strong acid inorganic acid generate a series of chemical reactions:
as is clear from the above chemical reaction formula, the precipitate formed by the reaction is silicic acid [ H]2SiO3↓](SiO2·nH2O) (also known as hydrated silica), aluminum silicate [ Al]2(SiO3)3↓]Calcium silicate [ CaSiO]3↓]Magnesium silicate [ MgSiO]3↓]And (4) precipitating. Separating the precipitate, washing with water, drying, dewatering and grinding to obtain precipitate mixture productThe invention names the product as 'silicon-aluminum-white'. The filtrate, i.e. mother liquor, is neutral with pH value of about 7 and contains only strong acidic inorganic sodium water solution and a small amount of excessive sodium silicate [ Na]2SiO3]A solution containing a sodium salt of a strongly acidic inorganic acid and a small excess of sodium silicate [ Na]2SiO3]And a dissolution amount of a neutral liquid in which four precipitated substances are main impurities. The neutralization treatment of the waste acid liquid is introduced by the water glass, so that the neutralization treatment and the comprehensive utilization of a large amount of soil waste acid liquid generated in the activated clay production can be unified, the problem can be solved in one step, and the environmental protection treatment cost in the activated clay production process is greatly reduced. The whole process is simple, high temperature and high pressure are not needed, and the new mixture, namely the silicon-aluminum-white product, produced by the invention has the characteristics of good activity, small apparent specific gravity, large specific surface area, oil absorption and water absorption. The product is a fine powder product with high whiteness, particularly light specific gravity and good chemical stability, and has the physicochemical characteristics that:
the white powder is insoluble in acid, soluble in hot concentrated alkali solution, insoluble in water and organic solvent, and resistant to oxidation and reduction agents. The components are as follows:
the water content is 4-8%
Silicon dioxide is more than or equal to 80 percent
Less than or equal to 4 percent of aluminum oxide
The whiteness is more than or equal to 90 percent
The residue on sieve (45 μm) is less than or equal to 0.5%
Apparent specific gravity of less than 0.4 g/ml
The total content of iron is less than or equal to 0.2 percent
The burning loss (950 ℃) is less than or equal to 7 percent
Therefore, the physical and chemical indexes of the product have the characteristics of high-market products such as white carbon black, ultrafine aluminum silicate salt particles, lithopone and the like, and the production cost is far lower than that of similar products. Can be used as active substances to be used as fillers and reinforcing agents of various materials such as rubber, plastics, paint, ink and the like; as suspending carrier and filler of white slurry preparation of pesticide; as a solidification preventive for deliquescent substances such as salt, fertilizers, agricultural chemicals, carriers for insecticides, and heat insulating materials; as white pigment, as solid filler of coating and paint; as industrial catalyst for petroleum refining; preparing a catalytic cracking agent carrier of petroleum and the like through proper pretreatment; used as the glaze batch ingredients for enamels, ceramics and porcelain utensils; used as the filler for white and colored rubber shoes, tires and rubber tubes; and the production cost is low, and the production process is simple. Most of the added aluminosilicate clay mineral becomes an activated clay product, and a small part of the aluminosilicate clay mineral becomes a silicon-aluminum white product, and a small amount of the aluminosilicate clay mineral is in the treated neutral wastewater; the trace amount of the strong acid inorganic acid is put into the activated clay product, the small amount of the strong acid inorganic acid is put into the silicon-aluminum white product, the large amount of the strong acid inorganic acid is put into the treated neutral wastewater in the form of salt, most of the water glass is put into the silicon-aluminum white product, the rest water glass is put into the treated neutral wastewater, the trace amount of the water glass is put into the product, the small amount of the water glass is dissipated into the atmosphere in the drying process of the product, and the large amount of the water glass is put into the treated neutral wastewater.
The object of the present invention can be further achieved by the following means. The method for treating and utilizing waste acid liquor of activated clay is characterized by that when the effective content of strong acid inorganic acid is measured, if its effective content per unit volume is less than 1.0 g/L, the strong acid inorganic acid or waste acid liquor with higher concentration is added into the waste acid liquor, and the effective content per unit volume is regulated to 1.0-50 g/L, then according to its effective content the water glass [ Na]is added2SiO3·nH2O]The reaction is carried out. Thus, the quality of the precipitation mixture product, namely the 'silica-alumina white' product, can be ensured.
The object of the present invention can be further achieved by the following means. The method for treating and utilizing the waste acid liquid of the activated clay is characterized in that the effective contents of the strong-acid inorganic acid are synchronously measured, and the effective contents of aluminum salt, magnesium salt and calcium salt of the strong-acid inorganic acid are measured. So as to more accurately calculate the amount of water glass added.
The object of the invention can also be achieved byThe following scheme is further achieved. The method for treating and utilizing the waste acid liquor of activated clay is characterized in that the waste acid liquor generated in the process of manufacturing the activated clay and sodium silicate [ Na]2SiO3]The temperature of the chemical reaction is 75-80 ℃. So that the reaction speed is higher and the quality of the precipitated mixture product is ensured.
Compared with the prior art, the method does not need the neutralization of quicklime or limestone, has simple treatment process and lower treatment cost, and the produced silicon-aluminum-white product has higheruse value. The process has no waste such as residue cake which can be discharged, and the treated neutral waste water is finishedThe single part of the aqueous solution only contains the sodium salt of the strong acid inorganic acid and a small amount of excess sodium silicate [ Na]2SiO3]Is a neutral liquid with main impurities. Can be further comprehensively utilized.
The attached drawing is a process flow chart of the invention.
The first embodiment. The following examples further illustrate the invention. The method for treating and utilizing the waste acid liquor of activated clay in this example is to use 0.5L of waste acid liquor generated in the production of activated clay from wet sulfuric acid activated aluminosilicate clay mineral, to sample and analyze the waste acid liquor, to determine that the effective content of sulfuric acid is 10 g, and to add water glass [ Na]with weight concentration of 52.69% according to the weight ratio of 1: 3.0 of the effective content2SiO3·nH2O]56.94 g of sodium silicate with 30 g of effective components, fully stirring and reacting with sulfuric acid, aluminum sulfate, magnesium sulfate and calcium sulfate in the waste acid liquor, wherein the waste acid liquor and sodium silicate [ Na]2SiO3]The temperature of the chemical reaction is 75-80 ℃, and silicic acid [ H]generated in the feed liquid after the reaction2SiO3↓]Aluminum silicate [ Al2(SiO3)3↓]Calcium silicate [ CaSiO]3↓]Magnesium silicate [ MgSiO]3↓]Separating out precipitate, washing with water, drying at 105 ℃, dehydrating and grinding to obtain 29 g of sediment mixture product, namely silica-alumina-silica-alumina, which has the characteristics that: containing silicon dioxide80.6 percent, 3.6 percent of aluminum oxide and 90 percent of whiteness, and the apparent specific gravity is 0.39 g/ml. The mother liquor only contains sodium sulfate and a small amount of excessive sodium silicate Na2SiO3]To a neutral aqueous solution of (a).
Example two. The following examples continue to illustrate the inventive content of the present invention. In the method for treating and utilizing the activated clay waste acid liquid in this embodiment, 0.5 l of waste acid liquid generated in the production of activated clay from wet sulfuric acid-activated aluminosilicate clay minerals is sampled and analyzed, and it is determined that the effective content of sulfuric acid is 10 g, the effective content of aluminum sulfate (calculated as aluminum oxide) is 0.432 g, the effective content of magnesium sulfate (calculated as magnesium oxide) is 0.206 g, and the effective content of calcium sulfate (calculated as calcium ions) is 0.184 g. Adding water glass [ Na]with the weight concentration of 52.69 percent according to the weight ratio of 1: 4.0 of the effective content of the sulfuric acid2SiO3·nH2O]75.92 g of sodium silicate with 40 g of effective component, fully stirring and reacting with sulfuric acid, aluminum sulfate, magnesium sulfate and calcium sulfate in the waste acid liquor, wherein the waste acid liquor and sodium silicate [ Na]2SiO3]The temperature of the chemical reaction is 75-80 ℃, and silicic acid [ H]generated in the feed liquid after the reaction2SiO3↓]Aluminum silicate [ Al2(SiO3)3↓]Calcium silicate [ CaSiO]3↓]Magnesium silicate [ MgSiO]3↓]Separating out precipitate, washing with water, drying at 130 ℃, dehydrating and grinding to obtain a precipitate mixture product, namely 30 g of silicon-aluminum white, which has the characteristics that: 84.8 percent of silicon dioxide, 3.5 percent of aluminum oxide and 94 percent of whiteness, and the apparent specific gravity is 0.31 g/ml. The mother liquor is 575.2 g, which only contains sodium sulfate and a small amount of excess sodium silicate Na2SiO3]To a neutral aqueous solution of (a).
Example three. The following examples continue to illustrate the inventive content of the present invention. The method for treating and utilizing the waste acid liquor of activated clay in this example is to use 0.5L of waste acid liquor generated in the production of activated clay from wet sulfuric acid activated aluminosilicate clay mineral, to sample and analyze the waste acid liquor, to determine that the effective content of sulfuric acid is 10 g, and to add water glass [ Na]with a weight concentration of 52.69% according to the weight ratio of 1: 4.5 of the effective content of sulfuric acid2SiO3·nH2O]85.41 g of sodium silicate with 45 g of effective component, fully stirring and reacting with sulfuric acid, aluminum sulfate, magnesium sulfate and calcium sulfate in the waste acid liquor, wherein the waste acid liquor and sodium silicate [ Na]2SiO3]The temperature of the chemical reaction is 75-80 ℃, and silicic acid [ H]generated in the feed liquid after the reaction2SiO3↓]Aluminum silicate [ Al2(SiO3)3↓]Calcium silicate [ CaSiO]3↓]Magnesium silicate [ MgSiO]3↓]Separating out precipitate, washing with water, drying at 150 ℃, dehydrating and grinding to obtain a precipitate mixture product, namely 35 g of silicon-aluminum white, which has the characteristics that: contains 81 percent of silicon dioxide, 2.85 percent of aluminum oxide and 94.9 percent of whiteness, and the apparent specific gravity is 0.29 g/ml. The mother liquor is 505 g, which only containssodium sulfate and a small amount of excessive sodium silicate [ Na]2SiO3]To a neutral aqueous solution of (a).
Example four. The following examples continue to illustrate the inventive content of the present invention. The method for treating and utilizing the waste acid liquor of activated clay in the embodiment comprises the steps of preparing the waste acid liquor of activated clay by using wet sulfuric acid to activate aluminosilicate clay minerals, sampling and analyzing the waste acid liquor, measuring the effective content of sulfuric acid, wherein the effective content per unit volume is 0.61 g/L, adding the waste acid liquor with the concentration of 53.51 g/L into the waste acid liquor, adjusting the effective content per unit volume to 1.0 g/L to obtain 10.61L of waste acid liquor, the effective content of sulfuric acid is 10.61 g, and adding water glass [ Na]with the weight concentration of 56.76% according to the weight ratio of 1: 5.6 of the effective content of sulfuric acid2SiO3·nH2O]104.68 g of sodium silicate with 59.42 g of effective component, fully stirring and reacting with sulfuric acid, aluminum sulfate, magnesium sulfate and calcium sulfate in the waste acid liquor, and mixing the waste acid liquor with sodium silicate [ Na]2SiO3]The temperature of the chemical reaction is 100 deg.CThe silicic acid [ H]generated in the feed liquid after the reaction is treated at the temperature of2SiO3↓]Aluminum silicate [ Al2(SiO3)3↓]Calcium silicate [ CaSiO]3↓]Magnesium silicate [ MgSiO]3↓]Separating out precipitate, washing with water, drying at 200 ℃, dehydrating and grinding to obtain 240.8 g of sediment mixture product, namely silicon-aluminum white, which has the characteristics that: contains 81.1 percent of silicon dioxide,3.08 percent of aluminum oxide, 90.8 percent of whiteness and 0.39 g/ml of apparent specific gravity. 2260 g of mother liquor is prepared by mixing sodium sulfate and a small amount of excessive sodium silicate Na2SiO3]To a neutral aqueous solution of (a).
Example five. The following examples continue to illustrate the inventive content of the present invention. The method for treating and utilizing the waste acid liquor of the activated clay comprises the steps of preparing waste acid liquor L of the activated clay by using wet sulfuric acid to activate aluminosilicate clay minerals, sampling and analyzing the waste acid liquor L, measuring the effective content of sulfuric acid, wherein the effective content per unit volume is 0.9 g/L, adding concentrated sulfuric acid into the waste acid liquor, adjusting the effective content per unit volume to 50 g/L to obtain 0.25L of waste acid liquor, the effective content of sulfuric acid is 12.5 g, and adding water glass [ Na]with the weight concentration of 52.69% according to the weight ratio of the effective content of sulfuric acid to 1: 5.02SiO3·nH2O]118.60 g of sodium silicate with 62.5 g of effective components, and the sodium silicate is fully stirred and reacted with sulfuric acid, aluminum sulfate, magnesium sulfate and calcium sulfate in the waste acid liquor, and the waste acid liquor is mixed with sodium silicate [ Na]2SiO3]The temperature of the chemical reaction is 20 ℃, and silicic acid [ H]generated in the feed liquid after the reaction2SiO3↓]Aluminum silicate [ Al2(SiO3)3↓]Calcium silicate [ CaSiO]3↓]Magnesium silicate [ MgSiO]3↓]Separating out precipitate, washing with water, drying at 130 ℃, dehydrating and grinding to obtain a precipitate mixture product, namely 69 g of silicon-aluminum white, which has the characteristics that: contains 83 percent of silicon dioxide and 2.80 percent of aluminum oxide, and has an apparent specific gravity of 0.39 g/ml. 1340 g of mother liquor containing only sodium sulfate and a small amount of excess sodium silicate Na2SiO3]To a neutral aqueous solution of (a).
Example six. The following examples continue to illustrate the inventive content of the present invention. The method for treating and utilizing the waste acid liquor of activated clay of the embodiment comprises the steps of preparing 0.7L of waste acid liquor generated by activated clay from aluminosilicate clay mineral activated by wet hydrochloric acid, sampling and analyzing the waste acid liquor, measuring that the effective content of hydrochloric acid is 9.352 g, and adding 52.69 wt% of water glass [ Na]according to the weight ratio of 1: 7.12 of the effective content of hydrochloric acid2SiO3·nH2O]126.3 g, wherein the effective component of the sodium silicate is 66.55G, mixing it with hydrochloric acid, aluminium chloride, magnesium chloride and calcium chloride in waste acid liquid, stirring them to react, and mixing the waste acid liquid with water glass [ Na]2SiO3]The temperature of the chemical reaction is 75-80 ℃, and silicic acid [ H]generated in the feed liquid after the reaction2SiO3↓]Aluminum silicate [ Al2(SiO3)3↓]Calcium silicate [ CaSiO]3↓]Magnesium silicate [ MgSiO]3↓]Separating out precipitate, washing with water, drying at 130 ℃, dehydrating and grinding to obtain 39 g of sediment mixture product, namely silicon-aluminum white, which has the characteristics that: 80.6 percent of silicon dioxide, 3.92 percent of aluminum oxide and 91.2 percent of whiteness, and the apparent specific gravity is 0.38 g/ml. 1390 g of mother liquor containing only sodium chloride and a small excess of sodium silicate Na2SiO3]To a neutral aqueous solution of(a).
Example seven. The following examples continue to illustrate the inventive content of the present invention. The method for treating and utilizing the waste acid liquor of activated clay of the embodiment comprises the steps of preparing 0.6L of waste acid liquor generated by activated clay from aluminosilicate clay mineral activated by wet nitric acid, sampling and analyzing the waste acid liquor, detecting that the effective content of nitric acid is 14.49 g, and adding 52.69 wt% of water glass [ Na]according to the weight ratio of 1: 4.24 of the effective content of nitric acid2SiO3·nH2O]116.55 g of sodium silicate with 61.41 g of effective component, reacting with nitric acid, aluminum nitrate, magnesium nitrate and calcium nitrate in the waste acid liquor by stirring, and mixing the waste acid liquor with water glass [ Na]2SiO3]The temperature of the chemical reaction is 75-80 ℃, and silicic acid [ H]generated in the feed liquid after the reaction2SiO3↓]Aluminum silicate [ Al2(SiO3)3↓]Calcium silicate [ CaSiO]3↓]Magnesium silicate [ MgSiO]3↓]Separating out precipitate, washing with water, drying at 130 ℃, dehydrating and grinding to obtain 39 g of sediment mixture product, namely silicon-aluminum white, which has the characteristics that: contains 81 percent of silicon dioxide, 3.72 percent of aluminum oxide and 91 percent of whiteness, and the apparent specific gravity is 0.37 g/ml. Its mother liquor 1190 g contains only sodium nitrate and small excess sodium silicate Na2SiO3]To a neutral aqueous solution of (a).
Claims (4)
1. The method for treating and utilizing the activated clay waste acid solution is characterized by comprising the following steps: samplingand analyzing the waste acid liquor produced by using wet-process strong acid inorganic acid to activate aluminosilicate clay mineral to make activated clay, measuring out effective content of its strong acid inorganic acid, adding sodium silicate Na as effective component according to the weight ratio of 1: 3.0-7.2 of effective content2SiO3]The water glass is fully stirred and reacted with strong acid inorganic acid in waste acid liquor and aluminum salt, magnesium salt and calcium salt of the strong acid inorganic acid at the temperature of 20-100 ℃, and silicic acid [ H]is generated in feed liquor after reaction2SiO3↓]Aluminum silicate [ Al2(SiO3)3↓]Calcium silicate [ CaSiO]3↓]Magnesium silicate [ MgSiO]3↓]Separating out precipitate, washing with water, drying at 105-200 deg.C, dewatering, and grinding to obtain precipitate mixture product, whose mother liquor only contains strong acid inorganic acid sodium salt and small amount of excessive sodium silicate [ Na]2SiO3]To a neutral aqueous solution of (a).
2. The method according to claim 1, wherein when the effective content of the strongly acidic inorganic acid is measured, if the effective content per unit volume is less than 1.0 g/l, the strongly acidic inorganic acid or the waste acid solution having a higher concentration is added to the waste acid solution to adjust the effective content per unit volume to 1.0-50 g/l, and then water glass [ Na]is added according to the effective content2SiO3·nH2O]The reaction is carried out.
3. The method according to claim 1, wherein the effective contents of the aluminum salt, magnesium salt and calcium salt of the strongly acidic inorganic acid are measured simultaneously with the measurement of the effective contents of the strongly acidic inorganic acid.
4. The process for the remediation of activated clay pickle liquor according to claim 1, wherein the activated clay is produced by the process of making activated clayThe waste acid liquid and water glass [ Na]2SiO3]The temperature of the chemical reaction is 75-80 ℃.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101638260B (en) * | 2009-09-04 | 2011-06-29 | 黄山市白岳活性白土有限公司 | Method for preparing polymeric aluminum sulfate silicate by recycling activated clay industrial wastewater |
| CN103030200A (en) * | 2013-01-09 | 2013-04-10 | 杨祺 | Method for producing poly-silicon rare earth chloride sulfate aluminum iron by using rare earth-containing sludge and electroplated and pickled acid-containing sewage |
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2000
- 2000-04-19 CN CNB001122231A patent/CN1142108C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101638260B (en) * | 2009-09-04 | 2011-06-29 | 黄山市白岳活性白土有限公司 | Method for preparing polymeric aluminum sulfate silicate by recycling activated clay industrial wastewater |
| CN103030200A (en) * | 2013-01-09 | 2013-04-10 | 杨祺 | Method for producing poly-silicon rare earth chloride sulfate aluminum iron by using rare earth-containing sludge and electroplated and pickled acid-containing sewage |
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