CN111762801A - Method for treating waste crystalline salt obtained by co-production of ethylene glycol and dimethyl carbonate - Google Patents
Method for treating waste crystalline salt obtained by co-production of ethylene glycol and dimethyl carbonate Download PDFInfo
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- CN111762801A CN111762801A CN202010587101.9A CN202010587101A CN111762801A CN 111762801 A CN111762801 A CN 111762801A CN 202010587101 A CN202010587101 A CN 202010587101A CN 111762801 A CN111762801 A CN 111762801A
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- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D9/00—Nitrates of sodium, potassium or alkali metals in general
- C01D9/04—Preparation with liquid nitric acid
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- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The invention belongs to the field of solid waste treatment, and particularly relates to a method for treating waste crystalline salt obtained by co-producing dimethyl carbonate with ethylene glycol, wherein the waste crystalline salt mainly comprises the following components: sodium nitrate, sodium carbonate, sodium oxalate, sodium formate and sodium nitrite, dissolving the waste crystal salt by water to obtain a waste crystal salt mixed solution, and sequentially carrying out the following treatment on the mixed solution: adding nitric acid, blowing air into the mixture at the temperature of 50-70 ℃, adjusting the pH of the mixed solution to be neutral, adding calcium hydroxide, filtering to remove precipitates, evaporating and crystallizing the filtrate, and drying to obtain a sodium nitrate product. According to the scheme provided by the invention, various components in the waste crystalline salt are converted into sodium nitrate through chemical reaction, most of by-products are gas or a small amount of precipitate in the reaction process, the by-products can be directly removed, and the obtained sodium nitrate product has high purity and can be directly used as industrial salt.
Description
Technical Field
The invention belongs to the field of solid waste treatment, and particularly relates to a method for treating waste crystalline salt obtained by co-producing dimethyl carbonate with ethylene glycol.
Background
Ethylene glycol is an important organic chemical raw material, is widely used for preparing polyester terylene, polyester resin, moisture absorbent, plasticizer, surfactant, synthetic fiber, cosmetics and explosive, is used as a solvent of dye/ink and the like, is used for preparing an antifreeze agent and a gas dehydrating agent of an engine, is used for preparing resin, and can also be used as a wetting agent of cellophane, fiber, leather and adhesive. The method for further producing the ethylene glycol and coproducing the dimethyl carbonate by using the coal synthesis gas is a novel technology for producing the ethylene glycol, has more advantages compared with the method for producing the ethylene glycol by using the petroleum as the starting material through an ethylene hydration method, becomes a large investment hotspot in recent years, and only China produces nearly 1000 million tons of ethylene glycol produced by the technology. However, in the process of manufacturing ethylene glycol by the process, a large amount of waste crystalline salt is generated, and it is estimated that in China, the amount of the waste crystalline salt generated by the process is nearly 10 ten thousand tons/year, the components are complex, the waste crystalline salt contains sodium nitrate, sodium carbonate, sodium oxalate, sodium formate, sodium nitrite and the like, and the waste crystalline salt is dangerous waste, and the waste crystalline salt is treated by adopting a solidification landfill mode in the current industry, so that the waste crystalline salt has two defects, namely, the waste of resources of a large amount of waste salt is caused; and secondly, the waste salt is extremely difficult to cure by adopting a conventional cement curing mode, the ratio of the waste salt to the cement is required to reach 1: 3-5 during curing, the curing effect is poor, and the waste salt is easy to leach out. Moreover, the "hazardous waste landfill pollution control Standard" (GB18598-2019), which was carried out since 1/6/2020, states that the total amount of water-soluble salts in hazardous waste must be less than 10% in flexible landfills, which is only an expedient even when entering rigid landfills, and that landfills are extremely costly. Thus, the landfill route of the waste salt is not feasible, and a new resource utilization way of the waste salt is required to be searched, so that sustainable development is realized.
Disclosure of Invention
The invention aims to provide a method for treating waste crystalline salt obtained by co-producing dimethyl carbonate with ethylene glycol, which converts other components in the waste crystalline salt into sodium nitrate by a chemical method, obtains a high-purity sodium nitrate product and avoids environmental pollution and resource waste caused by landfill disposal.
In order to achieve the purpose, the invention adopts the technical scheme that: a treatment method of waste crystallization salt obtained by co-production of ethylene glycol and dimethyl carbonate comprises the following main components: sodium nitrate, sodium carbonate, sodium oxalate, sodium formate and sodium nitrite, dissolving the waste crystal salt by water to obtain a waste crystal salt mixed solution, and sequentially carrying out the following treatment on the mixed solution: adding nitric acid, blowing air into the mixture at the temperature of 50-70 ℃, adjusting the pH of the mixed solution to be neutral, adding calcium hydroxide, filtering to remove precipitates, and evaporating and crystallizing the filtrate to obtain a sodium nitrate product.
By adopting the scheme, the added nitric acid solution can react with the sodium carbonate and the sodium formate in the mixture to convert the sodium carbonate and the sodium formate into sodium nitrate; blowing air at 50-70 ℃, wherein the oxygen in the air can oxidize the reductive sodium nitrite into sodium nitrate; after the pH value of the mixed solution is adjusted to be neutral, calcium hydroxide is added, and the mixed solution can react with sodium oxalate to generate calcium oxalate precipitate; filtering the mixed solution to remove precipitates, and carrying out evaporative crystallization treatment on the obtained filtrate to obtain a high-purity sodium nitrate product. According to the scheme provided by the invention, various components in the waste crystalline salt are converted into sodium nitrate through chemical reaction, most of by-products are gas or a small amount of precipitate in the reaction process, the by-products can be directly removed, and the obtained sodium nitrate product has high purity and can be directly used as industrial salt.
Specifically, the content of the waste crystalline salt obtained by co-producing dimethyl carbonate with ethylene glycol is generally as follows: 30-70% of sodium nitrate, 15-40% of sodium carbonate, 0-10% of sodium oxalate, 5-20% of sodium formate and 10-20% of sodium nitrite.
During treatment, the waste crystal salt and water are mixed in a ratio of 1: (1.0-2.0), slowly dropwise adding a nitric acid solution into the mixed solution at normal temperature, carrying out double decomposition reaction on the added nitric acid and sodium carbonate in the mixed solution, and converting the sodium carbonate into sodium nitrate:
Na2CO3+2HNO3＝2NaNO3+H2O+CO2↑
and (2) continuously dropwise adding a nitric acid solution, oxidizing the sodium formate which is a reducing salt with an aldehyde group structure into carbon dioxide to remove, contacting the produced nitric oxide with oxygen in the air to convert the nitrogen dioxide after the produced nitric oxide overflows as tail gas, and converting the nitrogen dioxide into nitric acid for recycling after the nitric oxide is absorbed by water through a tail gas absorption tower:
HCOONa+HNO3＝NaNO3+HCOOH
3HCOOH+2HNO3＝4H2O+3CO2↑+2NO↑
4NO+3O2+2H2O＝4HNO3
from the above equation, it can be seen that 2 moles of nitric acid are consumed for every mole of sodium carbonate and 5 moles of nitric acid are consumed for every 3 moles of sodium formate, and the amount of nitric acid added is at least the sum of the molar amounts of nitric acid consumed by the two substances, and may be slightly excessive but not less than this amount, so as to ensure the purity of the final sodium nitrate product. That is, the amount of nitric acid used is:
nnitric acid≥nSodium carbonate·2+nSodium formate·5/3
Wherein: n isNitric acidIs the amount of substance of nitric acid added, in mol;
nsodium carbonateThe amount of sodium carbonate in the waste crystal salt is unit mol;
nsodium formateThe amount of sodium formate in the waste crystallized salt is the unit mol.
The reaction of the nitric acid, the sodium carbonate and the sodium formate is exothermic, so that the temperature of the whole system is increased, the temperature of the reaction system can be controlled to be about 60 ℃ for ensuring the stable reaction, and the reaction system can reach the required temperature only by providing a small amount of heat in the subsequent process of removing the sodium nitrite through oxidation, thereby further reducing the energy consumption of the whole treatment process and reducing the treatment cost.
Blowing air into the reactor at the temperature of 50-70 ℃, preferably 55-65 ℃, and oxidizing sodium nitrite into sodium nitrate by oxygen in the air:
2NaNO2+O2＝2NaNO3
the blowing air speed is 0.1-0.3 m3(kg waste salt. h), the sodium nitrite content of the waste crystal salt is usually within the range of 10 to 20%, and air is blown for 1 to 3 hours, preferably 2 hours.
And (3) adjusting the pH value of the mixed solution to be neutral by adopting sodium hydroxide, adding calcium hydroxide, and reacting with sodium oxalate in the mixed solution to generate calcium oxalate precipitate:
Ca(OH)2+Na2C2O4＝CaC2O4+2NaOH
from the above equation, one mole of calcium hydroxide is consumed per one mole of sodium oxalate, and in order to ensure complete conversion of sodium oxalate to precipitate, the calcium hydroxide should be added in a slight excess, i.e., in an amount of the substance added to the calcium hydroxide greater than the amount of the substance in the waste crystalline salt.
And filtering the mixed solution to remove precipitate calcium oxalate and calcium hydroxide, wherein the obtained filtrate is the sodium nitrate solution. Evaporating, crystallizing, centrifugally dewatering and drying to obtain sodium nitrate product. Specifically, heating the obtained filtrate to volatilize water to obtain hot sodium nitrate concentrated mother liquor, cooling, reducing the temperature, reducing the solubility of sodium nitrate due to the reduction of the temperature, separating out crystals in the process of reducing the temperature, centrifugally dewatering, and drying the obtained crystals to obtain a sodium nitrate product.
According to the scheme, the impurity components in the waste crystallized salt are removed one by one through chemical reaction, and the reaction product is a gas discharge system or is finally filtered out for precipitation, so that a complex mixture is changed into single sodium nitrate, the purity of the obtained sodium nitrate solution is high, the purity of the sodium nitrate solution after evaporation and crystallization is up to more than 98%, the sodium nitrate solution meets the standard requirement of industrial sodium nitrate (GB/T4553-2016), the sodium nitrate solution can be directly used as industrial salt, and the resource utilization of the waste salt is realized. Compared with the curing and landfill process in the prior art, the curing and landfill treatment cost is saved by 5000-6000 yuan/ton, precious landfill resources are saved, and sodium nitrate can be sold as a product, so that the economic benefit and the environmental benefit are further improved.
Detailed Description
The technical solution of the present invention is further described below with reference to examples.
Example 1
The waste crystallized salt obtained by co-producing ethylene glycol and dimethyl carbonate consists of sodium nitrate 53.7 wt%, sodium carbonate 21.3 wt%, sodium oxalate 0.6 wt%, sodium formate 10.3 wt% and sodium nitrite 14.1 wt%.
Adding 30L of water and 20kg of waste salt into a 100L double-layer glass reactor, starting stirring for 15-30 minutes to dissolve, slowly dropwise adding 5.6kg of 60% industrial nitric acid into the reactor, releasing heat, reacting at the temperature of below 70 ℃ for 2-3 hours, converting sodium carbonate in the waste salt through double decomposition reaction, oxidizing sodium formate by nitric acid, and absorbing reaction tail gas by water.
Maintaining the temperature at 60 deg.C, adding 4m3Air was bubbled through the system at a rate of/h for about 2 hours to oxidize the sodium nitrite in the system to sodium nitrate.
After the pH value of the mixed solution is adjusted to be neutral by adopting sodium hydroxide, a small amount of slaked lime is slowly added for about 1kg for a plurality of times, and the stirring is continued for about 30 minutes, so that a small amount of sodium oxalate contained in the waste salt is converted into calcium oxalate precipitate, and the amount of the calcium oxalate precipitate is about 0.12 kg.
And (3) filtering the reaction liquid by adopting filter bag type filtering equipment, precipitating and filtering calcium oxalate, further heating to evaporate to remove part of water, cooling for crystallization, centrifugally dewatering and drying to obtain a product sodium nitrate of about 16kg, and returning the residual concentrated solution to the system to be circularly treated together with the waste crystallized salt mixed solution.
The purity of the sodium nitrate product is measured to be 98.5 percent and meets the standard requirement of industrial sodium nitrate (GB/T4553-2016).
Example 2
The waste crystallized salt for co-production of ethylene glycol and dimethyl carbonate consists of sodium nitrate 58.2 wt%, sodium carbonate 20.1 wt%, sodium oxalate 0.5 wt%, sodium formate 11 wt% and sodium nitrite 10.2 wt%.
Adding 25L of water and 20kg of waste salt into a 100L double-layer glass reactor, starting stirring for 15-30 minutes to dissolve, starting stirring, slowly dropwise adding 5kg of 68% industrial nitric acid into the reactor, releasing heat, reacting at the temperature below 60 ℃ for 2-3 hours, converting sodium carbonate in the waste salt through double decomposition reaction, oxidizing sodium formate by nitric acid, and absorbing reaction tail gas by water.
Further heating to 70 ℃ to a temperature of 4.5m3Air was bubbled through the system at a rate of/h for about 2 hours to oxidize the sodium nitrite in the system to sodium nitrate.
After the pH value of the mixed solution is adjusted to be neutral by adopting sodium hydroxide, a small amount of slaked lime is slowly added for about 1.04kg for many times, and the stirring is continued for about 30 minutes, so that a small amount of sodium oxalate contained in the waste salt is converted into calcium oxalate precipitate, and the calcium oxalate precipitate is about 0.1 kg.
And (3) filtering the reaction liquid by adopting filter bag type filtering equipment, filtering and removing calcium oxalate precipitate, further evaporating to remove part of water, cooling, crystallizing, centrifugally dewatering and drying to obtain a product sodium nitrate of about 15.6kg, and returning the residual concentrated solution to the system to be circularly treated together with the waste crystallized salt mixed solution.
The purity of the sodium nitrate product is measured to be 99.1 percent and meets the standard requirement of industrial sodium nitrate (GB/T4553-2016).
Example 3
The waste crystallized salt for the co-production of ethylene glycol and dimethyl carbonate consists of sodium nitrate 51%, sodium carbonate 22%, sodium oxalate 0.7%, sodium formate 12% and sodium nitrite 14.3%.
Adding 38L of water and 20kg of waste salt into a 100L double-layer glass reactor, starting stirring for 15-30 minutes to dissolve, starting stirring, slowly dropwise adding 6.8kg of 50% industrial nitric acid into the reactor, releasing heat, reacting at the temperature below 60 ℃ for 2-3 hours, converting sodium carbonate in the waste salt through double decomposition reaction, oxidizing sodium formate by nitric acid, and absorbing reaction tail gas by water.
Further heating to 65 ℃ and adding 4.8m of the solution3Air was bubbled through the system at a rate of/h for about 2 hours to oxidize the sodium nitrite in the system to sodium nitrate.
After the pH value of the mixed solution is adjusted to be neutral by adopting sodium hydroxide, a small amount of slaked lime is slowly added for about 1kg for a plurality of times, and the stirring is continued for about 30 minutes, so that a small amount of sodium oxalate contained in the waste salt is converted into calcium oxalate precipitate, and the amount of the calcium oxalate precipitate is about 0.14 kg.
And (3) filtering the reaction liquid by adopting filter bag type filtering equipment, filtering and removing calcium oxalate precipitate, further evaporating to remove part of water, cooling, crystallizing, centrifugally dewatering and drying to obtain a product sodium nitrate of about 14.8kg, and returning the residual concentrated solution to the system to be circularly treated together with the waste crystallized salt mixed solution.
The purity of the sodium nitrate product is measured to be 99.5 percent and meets the standard requirement of industrial sodium nitrate (GB/T4553-2016).
Example 4
The waste crystallized salt for the production of ethylene glycol and dimethyl carbonate consists of sodium nitrate 53.7 wt%, sodium carbonate 21.3 wt%, sodium oxalate 0.6 wt%, sodium formate 10.3 wt% and sodium nitrite 14.1 wt%,
30L of water, 18kg of waste salt and 4kg of crystallization mother liquor are added into a 100L double-layer glass reactor, stirring is started for 15-30 minutes to dissolve, stirring is started, 7.6kg of 40% industrial nitric acid is slowly dripped into the reactor, heat is released, the reaction is controlled below 60 ℃ for 2-3 hours, sodium carbonate in the waste salt is converted through double decomposition reaction, sodium formate is oxidized by nitric acid, and reaction tail gas is absorbed by water.
Further heating to 65 ℃ and pouring the mixture into the reaction solution at a temperature of 3.8m3Air was bubbled through the reaction mixture at a rate of/h for about 2.5 hours to oxidize the sodium nitrite in the system to sodium nitrate.
After the pH value of the mixed solution is adjusted to be neutral by adopting sodium hydroxide, a small amount of slaked lime is slowly added for about 1kg for a plurality of times, and the stirring is continued for about 30 minutes, so that a small amount of sodium oxalate contained in the waste salt is converted into calcium oxalate precipitate, and the amount of the calcium oxalate precipitate is about 0.11 kg.
And (3) filtering the reaction liquid by adopting filter bag type filtering equipment, filtering and removing calcium oxalate precipitate, further evaporating to remove part of water, cooling, crystallizing, centrifugally dewatering and drying to obtain a product sodium nitrate of about 15.6kg, and returning the residual concentrated solution to the system to be circularly treated together with the waste crystallized salt mixed solution.
The purity of the sodium nitrate product is measured to be 98.3 percent and meets the standard requirement of industrial sodium nitrate (GB/T4553-2016).
Claims (7)
1. A treatment method of waste crystalline salt obtained by the coproduction of ethylene glycol and dimethyl carbonate is characterized in that: the waste crystalline salt mainly comprises the following components: sodium nitrate, sodium carbonate, sodium oxalate, sodium formate and sodium nitrite, dissolving the waste crystal salt by water to obtain a waste crystal salt mixed solution, and sequentially carrying out the following treatment on the mixed solution: adding nitric acid, blowing air into the mixture at the temperature of 50-70 ℃, adjusting the pH of the mixed solution to be neutral, adding calcium hydroxide, filtering to remove precipitates, and evaporating and crystallizing the filtrate to obtain a sodium nitrate product.
2. The method for treating the waste crystalline salt obtained by the coproduction of ethylene glycol and dimethyl carbonate according to claim 1, which is characterized in that: 30-70% of sodium nitrate, 15-40% of sodium carbonate, 0-10% of sodium oxalate, 5-20% of sodium formate and 10-20% of sodium nitrite.
3. The method for treating the waste crystalline salt obtained by the coproduction of ethylene glycol and dimethyl carbonate according to claim 1, which is characterized in that: the mixed solution is prepared by mixing waste crystal salt and water 1: (1.0-2.0) in a weight ratio.
4. The method for treating the waste crystalline salt obtained by the coproduction of ethylene glycol and dimethyl carbonate according to claim 1, which is characterized in that: the dosage of the nitric acid is as follows:
nnitric acid≥nSodium carbonate·2+nSodium formate·5/3
Wherein: n isNitric acidIs the amount of substance of nitric acid added, in mol;
nsodium carbonateThe amount of sodium carbonate in the waste crystal salt is unit mol;
nsodium formateThe amount of sodium formate in the waste crystallized salt is the unit mol.
5. The method for treating the waste crystalline salt obtained by the coproduction of ethylene glycol and dimethyl carbonate according to claim 1, which is characterized in that: the blowing air speed is 0.1-0.3 m3V (kg waste salt. h), air is usually blown in for 1 to 3 hours.
6. The method for treating the waste crystalline salt obtained by the coproduction of ethylene glycol and dimethyl carbonate according to claim 1, which is characterized in that: and (3) adjusting the pH of the mixed solution to be neutral by adopting sodium hydroxide, wherein the amount of substances added with calcium hydroxide is larger than that of the substances added with sodium oxalate in the waste crystallized salt.
7. The method for treating the waste crystalline salt obtained by the coproduction of ethylene glycol and dimethyl carbonate according to claim 1, which is characterized in that: and the evaporative crystallization is to evaporate, crystallize, centrifugally dewater and dry the filtrate to obtain a sodium nitrate product.
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Address after: 231100 Hefei, Anhui 231100 Patentee after: Anhui Haoyue Environmental Technology Co.,Ltd. Address before: 231145 Jinggang village, Wushan Town, Changfeng County, Hefei City, Anhui Province Patentee before: ANHUI HAO YUE ENVIRONMENTAL TECHNOLOGY Co.,Ltd. |